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By John Wulff, David A. Stevenson

The solubility of iron and cobalt in liquid lead, the solubility of chromium in liquid tin, and nickel in liquid silver were determined up to 1300°C in an atmosphere of hydrogen. Liquid samples were taken at different temperatures and analyzed. The data obtained were plotted to show the relationship between log mole fraction of solute and the inverse of the absolute temperature. Resulting values for the differential heat of solution (AH) and the excesspartial molar entropy (S)are: for the iron-lead system = _24,200 cal per mole and AT = 5.0 e.u. for the a phase, and AH = 18,300 and S = -0.1 e.u. for the y phase; for the cobalt-lead system AH = 16,500 cal per mole and AS =0.7 e.u.; for the chromium-tin system AH = 15,600 cal per mole and AS = 8.5 e.u.; for the nickel-silver system AH =18,000 cal per mole and AS = 4.0 e.u. RECENT developments in coating, brazing, and heat transfer have focused attention on specific cases of solid-liquid interaction in metal systems, particularly those involving dilute liquid solutions. One fundamental quantity of interest in such systems is the equilibrium phase distribution between solid and liquid phases. In any effort to fully understand such interactions, one must be able to describe the equilibrium state precisely. Furthermore, in order to develop genera! relations for such systems, one must know the equilibrium state in a number of different cases. This investigation was devoted to a study of the equilibrium phase distribution in four binary systems: solid iron-liquid lead; solid cobalt-liquid lead; solid chromium-liquid tin; solid nickel-liquid silver. The iron-lead system was previously studied by Shepard and parkman' and later by Fleischer and Elliott2 with differing results. Both investigations were carried out by sampling the saturated liquid, and analyzing it chemically. The cobalt-lead system was previously reported by Pelzel,3 who noticed no discontinuity near the transformation. A limited investigation of the chromium-tin system was made by Wlodek and wulff4 using a weight loss method. This work was done in conjunction with the development of a process for coating molybdenum with chromium from tin solutions. To more fully under- stand the kinetics of the process, a more accurate determination of a solubility was desirable. No significant data were found in the literature on the nickel-silver system. Data on the latter system were, however, relevant to the investigation of the corrosion kinetics of copper-nickel alloys in liquid silver as carried out by Harrison and wagner,5 EXPERIMENTAL APPARATUS AND PROCEDURE Of the techniques available for the study of such systems the most effective appears to be that of liquid sampling,2,6,7 which is the method used in the present investigation. A schematic diagram of the sampling furnace is given in Fig. 1. Large pieces of solute metal, in excess of saturation solubility, were added to 200 g of the solvent metal, and the entire charge placed in an alundum crucible. Analytical reagent or materials of chemically pure grade were used in all investigations. The crucible was contained in a zircon muffle tube positioned vertically in the uniform hot zone of a Globar resistance furnace. The tube was provided with a number of ports which permitted sampling at temperature and in controlled atmospheres or vacuum; the ports were also useful for evacuation and introduction of gases as well as for thermocouple measurements. A chromel-alumel thermocouple Sheated in a porcelain tube was used for temperature measurements. A purified hydrogen atmosphere was employed in all experiments reported in this paper. The hydrogen was purified by passing it first over hot copper gauze to remove oxygen and then through a molecular sieve immersed in

Jan 1, 1962

By T. C. Clarke

The history of iron construction in this country well illustrates the three phases of thought described by Auguste Comte, the French philosopher. The first is the era of faith, when belief in the safety of structures rests on the authority of the designer. The second is the era of criticism, when plans of structures are analyzed with much mathematical skill, but the data upon which the chain of reasoning depends is assumed upon insufficient experiment. The third, upon which we are now entering, is a scientific era, which demands experimental proof. It also demands that this proof shall be derived from experiments made on full-sized specimens, such as are in actual use, and not upon toy models. Until the construction of the United States testing-machine, now at Watertown Arsenal, it was impossible to make such experiments with accuracy. We now have a machine in which we can test full-sized specimens of every part of a bridge or other structure that we want to use, and under the same conditions in which it is actually used. The next thing is to get money to make these experiments available. No private individuals can afford to do it, and even if they could, they might wish to keep the results to themselves. So that the next point is that we want money, and that, I believe, everybodly thinks we should ask Congress for. We want also, as has been said, some one who shall make a business of testing, and who has plenty of time. Persons who are employed in private business are too much in a hurry; they want to do a thing and get done with it, and then do something else; but government officers are entirely free from this feeling; time to them is of no account, and in experimenting that is the very element that is of value; it does not do to be hurried; the great thing is to get it right and to test your results, and go over it, again and again. And the experimenter who operates the machine must be some person educated up to the use of it. We then want a general advisory board who will indicate a plan of experiments, collect the results; and publish them. Some experiments were made the other day at the Watertown Arsenal upon full-sized

Jan 1, 1882

By E. D. Leavitt

I desire to state briefly my views respecting the great practical value of the Watertown testing-machine, and the necessity that exists, for an able permanent commission to supervise its operations, in order that the results of all tests made thereon may be properly worked out and rendered available for public use. It is doubtless known to the Institute that this machine has, for the past two years, been placed at the service of the public upon payment of a per diem charge. It was my privilege to be among the first to use the testing-machine, and the results of my first experiments were of such importance, owing to the great capacity and extreme accuracy of the machine, that it has since become my practice to have tests of all materials used in constructions that came under my charge, made at Watertown. As a conseqnence, nearly one hundred tests have been made on my account directly, and some two hundred and forty additional for work built from my designs. It may be confidently affirmed, that the factor of anxiety on all these structures is exceedingly small .m far as the quality of material is concerned, and it is undoubtedly a very great advantage for parties interested in construction to have

Jan 1, 1882

By Ashbel Welch

Gentlemen of the American Institude of Mining Engineers.—As you well know an application is about to be made to Congress, by the American Society of Civil Engineers, for the appointment of a cornmission composed of persons skilled in the production and use of iron, steel, and other structural materials, whose duty it shall be to test the strength, elasticity, and other quatities of such materials ; not simply the substances used as such, but the members of large structures composed of such materials, of the forms and sizes in which they are actually used. As I understand, the papers that will be read here to- night will have for their object to show the necessity for such tests, and therefore the necessity for the commission asked for. As the representative of the Society of Civil Engineers, I have to thank you, gentlemen of the Mining Engineers, for the great zeal with which yon have taken up this subject, and seconded the efforts of the Civil Engineers; or, perhaps I ought rather to say, initiated the efforts to get a suitable commission appointed to obtain most vitally important information which it is admitted on all hands we do not now posses. In drawing up the memorial to Congress, in connection with some of the ablest and best informed of our Society, and in all the discossions on the subject, I have been struck with the emphasis with which the confession is made, that so little is known of the strength of the larger-sized members constantly used in building structures of the magnitude which the present requirements of the country now demand. I presume the remarks made to-night will bring this out very prominently. This is no disgrace, for with the means here-

Jan 1, 1882

By F. M. Lewis, J. F. Meyers

This second progress report of grinding presents comments regarding ball consumption and data pertaining to the hydroscillator, which is closed circuited with the tricone mill. A study and postulate of how balls function is presented. The paper summarizes cost reduction obtained by the method of "grinding for the tail race" rather than for "mesh tons." AT the Regional meeting in Columbus, Ohio, in September 1949, the authors presented a progress report of the first year's operation with a Hardinge tricone mill in closed circuit with a Dorr hydroscillator. The present report covers our findings on this grinding circuit to January, 1950. In order to clarify our position, the authors wish to state that no invention or discovery is claimed. The Tennessee grinding circuit is simply an engineered arrangement of known equipment arranged to incorporate all of the recognized efficiency factors of comminution as they are known today. As we concluded our first report, it was not clear how effective the Tennessee mode of operation would be on harder ores. The only information we had at that time was that the Bond grindability test at 48-mesh gave 6.04 g of undersize per revolution. A later test on the same sample at 100-mesh reduced this to 2.04 g, which is definitely in the harder ore class, and which makes the reported 8.80 kw-hr per ton of —200-mesh produced a very creditable figure. Hydroscillator Operation The machine as now developed has proved dependable and easy to operate. It starts easily under full load and responds quickly to operating adjustments. The hydraulic holes in the oscillating plate do not plug when shut down under full load. Absolutely clean hydraulic water is essential. An Elliott water screen or similar device should be an essential part of the machine to keep all scale and trash of all kinds from the hydraulic compartment. The shift operators have expressed approval of the machine. In table I we show a typical screen analysis of the hydroscillator rake sand as compared to conventional classifier rake sand on our ore. We have previously reported that of the 28.7 pct reduction in power, the hydroscillator contributed 6 pct, on a —200-mesh basis. This is a conservative figure. Some of our test runs indicated that the saving was as high as 10 pct. Laboratory studies by the Dorr Co. engineers indicate that still greater efficiency is possible. Nevertheless, the 10-ft plate is overflowing 2100 tons per day at 3 to 4 pct + 65-mesh, which is a very creditable performance by

Jan 1, 1951

By F. M. Lewis, J. F. Meyers

This second progress report of grinding presents comments regarding ball consumption and data pertaining to the hydroscillator, which is closed circuited with the tricone mill. A study and postulate of how balls function is presented. The paper summarizes cost reduction obtained by the method of "grinding for the tail race" rather than for "mesh tons." AT the Regional meeting in Columbus, Ohio, in September 1949, the authors presented a progress report of the first year's operation with a Hardinge tricone mill in closed circuit with a Dorr hydroscillator. The present report covers our findings on this grinding circuit to January, 1950. In order to clarify our position, the authors wish to state that no invention or discovery is claimed. The Tennessee grinding circuit is simply an engineered arrangement of known equipment arranged to incorporate all of the recognized efficiency factors of comminution as they are known today. As we concluded our first report, it was not clear how effective the Tennessee mode of operation would be on harder ores. The only information we had at that time was that the Bond grindability test at 48-mesh gave 6.04 g of undersize per revolution. A later test on the same sample at 100-mesh reduced this to 2.04 g, which is definitely in the harder ore class, and which makes the reported 8.80 kw-hr per ton of —200-mesh produced a very creditable figure. Hydroscillator Operation The machine as now developed has proved dependable and easy to operate. It starts easily under full load and responds quickly to operating adjustments. The hydraulic holes in the oscillating plate do not plug when shut down under full load. Absolutely clean hydraulic water is essential. An Elliott water screen or similar device should be an essential part of the machine to keep all scale and trash of all kinds from the hydraulic compartment. The shift operators have expressed approval of the machine. In table I we show a typical screen analysis of the hydroscillator rake sand as compared to conventional classifier rake sand on our ore. We have previously reported that of the 28.7 pct reduction in power, the hydroscillator contributed 6 pct, on a —200-mesh basis. This is a conservative figure. Some of our test runs indicated that the saving was as high as 10 pct. Laboratory studies by the Dorr Co. engineers indicate that still greater efficiency is possible. Nevertheless, the 10-ft plate is overflowing 2100 tons per day at 3 to 4 pct + 65-mesh, which is a very creditable performance by

Jan 1, 1951

Jan 1, 1896

By Franklin J. Hill, Theodore D. Tiemann

Sized fractions of Wisconsin Gogebic taconite were reduced with hydrogen over the temperature range from 600° to 1000°C. In general, the degree and rate of reduction increase with temperature. Particle size has no observable effect except in the smaller fractions at 900°C and above, where reduction is impeded, possibly due to the siliceous nature of the ore. Gaseous diffusion appears to be significant as a rate controlling factor at certain stages. THE depletion of high grade iron ore reserves in the United States has established the need to utilize all available iron ore deposits, both in long range planning and from the viewpoint of national emergency. This has led to extensive research and development in this field. The beneficiation of Wisconsin Gogebic taconite ore has been previously studied by investigators at the University of Wiscconsin, 1 the United States Bureau of Mines,, Battelle Memorial Institute, 3 and others. Methods investigated have included concentration by flotation processes, magnetic and gravity separation, magnetic roasting and various combinations of them. The foregoing studies have been concerned with the production of an enriched ore suitable for blast furnace use. If the ore could first be reduced to metallic iron and then beneficiated, the product could be used directly in the open hearth or electric steel-making furnace. The by-passing of the blast furnace should enhance the economic feasibility of the beneficiating process. The work reported here,4 was undertaken to establish data on the hydrogen reduction of Wisconsin taconite that would eventually lead to the development of an economic direct reduction process for this and perhaps other low grade siliceous ores. The volume of work on direct reduction can be judged by the fact that 240 direct reduction processes were patented in the United States alone up to 1951, 5 and numerous additional processes have since been developed. Some of the factors contributing to direct reduction development are: 1) The increasing capital cost of the blast furnace and its accessory equipment. 2) The decreasing availability of high grade domestic ore. 3) The high cost of steel scrap for use in the open hearth and electric furnaces. In general, direct reduction processes can be divided into two types; those using a solid reductant (coal, peat, lignite) usually carried out in a kiln, and those using a gaseous reductant (H2, CO) in a shaft furnace or a fluidized bed retort. As there is no low cost coal readily available in northern Wisconsin but natural gas could be quite easily obtained, it is believed a gaseous reductant process would offer the greater feasibility for use on Wisconsin taconite. It is hoped that this preliminary work will beof interest to other investigators in this increasingly important field. TACONITE ORE The ore used in the investigation was obtained originally from the U. S. Bureau of Mines, and consisted of a representative composite made up from trench samples of the Norrie, Pabst, Plymouth, Pence, and Yale members of the Wisconsin Gogebic range iron formation. Chemically, the ore contains approximately 52 pct SiO, and 30 pct Fe. X-ray diffraction and other studies indicate the principal minerals to be quartz (SiO2), hematite (Fe2O3), and goethite (Fe2O3. H2O). Minor amounts of iron containing silicates, siderite (FecO3), and magnetite (FeO-Fe2O3) are present. The iron minerals and quartz are so finely disseminated that the ore requires grinding to less than 200 mesh (74 µ) for essential liberation.l,2 The iron content of each of the several size fractions studied is shown in Table I. EXPERIMENTAL METHOD The method used throughout the investigation was based on that developed by the U. S. Bureau of Mines in Minneaopolis6,7 in which the course of reduction is followed by the loss in weight of the ore sample. More specifically, a 100-g sample of the size frac-

Jan 1, 1962

By I. L. Dillamore

I. L. Dillamore (University of Birmingham)—The different textures developed in various fcc metals have long awaited satisfactory explanation and it has now become clear that these differences are related to parallel differences in the deformation characteristics of the metals. Liu is correct, therefore, in seeking to account for the observed textures in terms of the flow mechanisms but I believe, for the reasons outlined below, that the particular interpretation of flow mechanisms proposed by Liu is open to substantial objections. By considering the forty-eight possible designations of the twelve octahedral slip systems found in fcc metals as distinct and separate deformation modes, Liu has fallen into the error of assuming that only positive glide dislocations associated with each system are present. In fact both positive and negative dislocations will be present and the only difference between for instance the systems B4 and B4' (in Liu's notation) is that under a stress of given sign the direction of motion of a dislocation is reversed on changing from B4 to B4'. For both orientations positive and negative dislocations will be present. In considering possible dislocation interactions it is, therefore, inadmissible to differentiate between R4 and R4' as Liu does. Liu considers those dislocation interactions which give the biggest reduction in energy to be the most favorable and neglects, on the grounds that they will form strong barriers to slip, interactions between dislocations with perpendicular Burgers vectors. Setting aside interactions between positive and negative dislocations of the same slip system, which must occur regardless of the combination of slip systems chosen, the biggest reduction in energy occurs for the Lomer-Cottrell interaction and it is Lomer-Cottrell barriers which are thought to provide the stronger dislocation obstacles. On the other hand the intersection of dislocations with perpendicular Burgers vectors is thought to be a low-energy process which contributes only a fairly small temperature-dependent part of the total work hardening. On this basis it seems doubtful whether the reduction in energy through possible dislocation interactions provides a reasonable criterion for choosing the operative slip systems. From the point of view of texture development it is unsatisfactory to ignore the slip rotations leading to an end position and to neglect to consider the stability of the chosen end point. It is also unsatisfactory to treat the two stress axes as interchangeable since, if the stress system is idealized as biaxial, one stress is compressive and the other is tensile. For the same reason the rotations of the two stress axes are not made compatible simply by assuming that the same slip directions are responsible for the rotations of the two stress axes. It is, in short, essential to treat the two stress axes as acting together on the same slip systems. Turning to the question of the difference between the copper-type and the brass-type texture, there now remains little doubt that the difference is attributable to differences in stacking-fault energy (y), as noted by Liu, but it is doubtful whether the temperature dependence of the texture in copper and in silver is due to increasing stacking-fault energy with increasing temperature. The results of Swann and Nutting42 cited by Liu were obtained in Cu-A1 alloys and the apparent increase in stacking-fault energy on raising the temperature may be influenced by short-range ordering. In pure metals such effects are absent and the only data available on the variation of y with temperature are those of Buhler et a1.43 for silver. They report a minimum at 200°C which does not fit the hypothesis put forward by Liu. It is much more likely that thermal activation of cross slip is important in determining which texture develops, as proposed by Dillamore and tors. These workers have proposed an explanation for the differences in observed texture among the fcc metals and the pole figures predicted consist of an orientation spread which is in better agreement with observation than the limited number of discrete orientations suggested by Liu. The theory of Dillamore and Roberts is also able to account for the differences between aluminum and copper which Liu still leaves unexplained. Y. C. Liu (author's veply)—The writer appreciates the interest of Dr. Dillamore, but must discuss some of his comments in order to avoid cross purposes. The phrase, "forty-eight slip systems," which appeared twice in the text—in the caption of Fig. 1 and the first paragraph in the Discussion—might unfortunately have led Dr. Dillamore to disagree

Jan 1, 1965

By John B. Pearse

IN order to get an idea as to the strength of steel rails, it will be well to review the tests to which iron rails have been subjected. In England, Mr. Ashcroft found that the best 80 pound rails broke under a 300 pound weight, falling 15 feet. In Germany the Society of Railway tyfanage1-s determined 011 and have long applied a test of 1000 pounds falling 101/2 feet, as the standard which all first-class iron rails must reach. In this country no inspection nor test is applied, but tests made show that iron rails fro; our most reliable makers, break under a G foot fall of a 1500 pound drop as an extreme test, most of those tested breaking under a far less test; some breaking with less than a 3 foot fall of the same weight. Everywhere where steel has been used, engineers have come to the conclusion that some test is required to show the regularity and strength of the product. As compared with iron, the tests which steel will stand are wonderful. After numerous experiments partially based on the experience of the rail-mill at Graz, belonging to the Southern Railway of Austria, the Society of German Railway Managers fixed upon a test of 2000 pounds falling 138 feet. They found that this test represented the steel which suited their necessities, and also found that with steel of otherwise average purity, this test represented about one-half per cent. of carbon, and made it a rule to take no steel containing under three-tenths of a per cent. of carbon, because it was too soft. They expressed a hope that a harder steel could soon be made tough enough to stand the same test. I n England, a test was adopted of 2240 pounds, falling 15 to 17 feet on the rail on heavy bearings. This test has been found satisfactory under heavy traffic on average road-beds, and has been invariably

By Sir Robert Hadfield

Introduction.-I esteem it a great honor to be asked by this Institute to give them an address chiefly devoted to metallurgy. While it is with great regret that I find myself unable to be present to deliver this in person, I take this opportunity of wishing your society every success in its continued career of usefulness to the metallurgists of the great Republic. To be elected, eight years ago, along with Dr. J. E. Stead, F. R. S., as one of your Honorary Members, was a privilege which I greatly esteemed, for I consider that no society in America has done so much as ours for the advancement of metallurgy. Those who have Served our Society.-Where many have served so well, it is difficult, without appearing to make unavoidable distinctions, to select names from those of your members who have done so much for the cause we have at heart-the advance and progress of metallurgy. As typical, however, and not in any way meant as a complete list, there are among others the following names which in the past and to-day stand out prominently in this science of ferrous metallurgy. With most of those now mentioned I have personally come in contact, or by correspondence in some few cases, and have exchanged views, since I first came over to America 30 years ago. Holley; Jones; Weeks; Andrew Carnegie; Thomas Carnegie; Fritz; Sterry Hunt;. Egleston; Maunsel White and Taylor, who did so much for high-speed tool steel, and helped to revolutionize machine-shop practice; W. J. Taylor; Robert Hunt; Alfred Hunt of Pittsburg, who did so much in the early history of aluminum, and, alas! did. not live to see the wonderful progress which has been made in that particular branch of metallurgical industry; James Douglas; C. B. Dudley; Birkinbine; Howe; Metcalf; Barus; Langley; Raymond; P. H. Dudley; H. H. Campbell; W. R. Webster; E. D. Campbell; Talbot; Spilsbury; Gayley; Dinkey, under whose supervision and responsibility modern armor has been so successfully produced in this country, which the writer can testify from personal knowledge of , test results possesses very high Figure of Merit; Schwab; Kennedy; Wellman; Garrison; Wood; Moldenke; Webster; Swank; Unger; Richards; Sauveur; Strat-

Jan 5, 1914

By Edward Keller

Although the subject matter contained in this paper is presented under a new title, its writing was induced by the work of S. Skowronski and K. W. McComas.' A discussion of the latter is here combined with the presentation of new and independent data. The' physical constants quoted by the authors of that paper, such as melting and boiling points, as also the chemical reactions of the substances involved, are so well established that the numerous confirmatory experiments and their application to metallurgical conditions leave little or no room for criticisms. On the contrary, they will greatly aid to dispel any lingering skepticism as to possible considerable losses of copper accruing when the metal is melted in the presence of its own and, probably, other chlorides and when no provision is made for the recovery of volatile products. Exception may be taken, to some degree, to that part of the work under the caption Melting Drillings of Copper Mixed with Sodium Chloride. These experiments should have been extended in order to make the implied reactions clear and the results convincing. The latter are stated to be, "that when sodium chloride is present above certain minimum quantity relative to copper some of it is found to volatilize in the melt while another part reacts with the metallic copper to produce the volatile cuprous chloride, and that when smaller quantities of sodium chloride are present the reaction is complete and all chlorine is found to have volatilized as cuprous chloride." Metallic copper and sodium chloride are mentioned as the sole reagents in this chemical process, acting, according to the authors, in a neutral atmosphere of carbon dioxide. The chemist, quite naturally, wi11 inquire into the formula according to which that reaction takes place and will find that it presents itself as follows: 2Cu + 2NaCl = 2Na + Cu2Cl2 It would appear that the truth of this formula will be challenged and a more rational explanation of the reaction sought. Apparently, carbon dioxide is neutral relative to metallic copper in its molten state; whether it remains neutral in the presence of sodium chloride is quite another

Jan 1, 1921

By J. K. Kerver, J. S. Osoba, J. G. Richardson, J. A. Hafford

A detailed study of a number of methods of relative permea-abilitv measurement has been made in a search for the tech-niqrle most suited to routine analysis of cores taken from reservoir rock. It has been found from tests run on the same samples of core material by a number of techniques that the Penn State, Hassler, Hafford, and dispersed feed techniques all yield results which are felt to be reliable. Conditions under which the faster single core dynamic technique may be used are described. Further work on the calculation of relative permeabilities to oil from data obtained by the gas drive method is needed before this latter rapid method can be utilized. Correlations between theoretical studies and experimental results have been obtained in studies of the boundary effect. pressure distribution in two-phase flow, and gas expansion effects. Previous conclusions that the effects of the outflow boundary could be made negligibly small have been substantiated. Results of experimentally determined oil and gas pressure distributions along a core sample during flow are presented. Further studies of the effects of rate of flow in the measurement of relative permeability-saturation relations have shown that results are independent of the rate of flow as long as the flow rate is below the point where inertial effects commence. An analysis of the effects of a severalfold expansion of gas along the flow path indicates that while saturation gradients are induced in the test sample, the errors caused by this phenomenon in relative permeability measurements are small. INTRODUCTION Many pages of literature have been devoted to pointing out the need for relative permeability-saturation relations in reservoir engineering. One of the most attractive ways of obtaining this information is by the analysis of samples of core material taken from the formation in question, and again literature has described man); methods for obtaining these data. It is the purpose of this paper to present the work that has been done in the study of some of these published methods together with some other methods that have been recently developed in this laboratory. Also, a study of some of the factors that influence the laburatory determination of relative permeability-saturation relations is presented. FACTORS WHICH AFFECT LABORATORY STUDY OF FLUID FLOW THROUGH RESERVOIR ROCK To determine relative permeability-saturation relations of samples of reservoir rock in the laboratory, it is important to know what factors affect these measurements in order that the magnitude of these effects can be ascertained and steps then can be taken to eliminate or, in some cases, to minimize them. The factors that have been investigated are the boundary effect, the effect of gas expansion. and the rate effect. Boundary Effect In laboratory experiments in which two immiscible fluids are flowed through a porous medium, there exists a discontinuity of capillary properties at the outflow face. This discontinuity exists became the fluids pass from a region of finite capillary pressure in the sample to a region of zero capillary pressure in an open receiving vessel. The capillary forces existing in the core caupe the rock to tend to retain

Jan 1, 1952

By General Meigs

I do not know that I can do any more than to express my entire concurrence in the views which have. been already expressed by Mr. Macdonald. It appears to me that he has we over the wholz subject. I might add in regard to appealing to the Govern-

Jan 1, 1882

By W. C. Knopf, I. M. LeBaron

In the Carlsbad area potash is dry-mined and wet-concentrated. Wet concentration involves recircu-lation of saturated brines, with resultant difficulties of brine disposal and inherent losses in recovery through solution of the KCl. A dry beneficiation process for potash minerals would offer many advantages over present methods. International Minerals & Chemical Corp. has been working on development of a dry process for some time. This article is a progress report. Potash ores available in this country are largely mixtures of halite and sylvite contaminated with slimes and often with many sulfate and magnesium minerals. Electrostatic concentration of KCl when the contaminating minerals are in low percentage has been accomplished. Continuous production of better than 60 pct K2O concentrate from high potassium sulfate ores has not been demonstrated at the present time. Laboratory Procedure: Laboratory work on electrostatic beneficiation of potash minerals has been carried out using both pure crystals and mined ore. Electrostatic separation of the two main components of potash ore, sylvite (KCl) and halite (NaCl), is accomplished by first heat-treating the ore to allow for electric charging of the particles. Preferential exchange of' electrical charges between different mineral particles through surface contact is the principal mechanism involved. After proper conditioning of the particle surfaces, the oppositely charged minerals are dropped vertically into a horizontal electric field having a field gradient from about 5000 to 15,000 v per in. The particles are free-falling in the field. A suitable power supply is used to produce the proper total voltage for the electric field. Total required voltage is, of course, a function of electrode spacing. A typical electrode arrangement with power supply is shown in Fig. 1. In general, the total voltage on any system is 75,000 to 90,000 v. Power consumption is negligible, as leakage at insulators and corona discharge are the main losses in the system. Optimum preheat temperatures for pure material components generally are not the same as for mined minerals. Fig. 2 shows clearly that maximum recovery on a 50 pct pure KCl, 50 pct pure NaCl mixture occurs at a preheat temperature of about 600°F. In this test the preheat mixture was allowed to cool to about 225°F before dropping through the electric field. The optimum temperature for sep- aration is practically never the optimum temperature of preheat. Optimum separation for mined Carlsbad potash ores occurs when a preheat temperature closer to 900°F is used, as shown by Fig. 3, which plots percent sylvite (KCl) in the concentrate and tails as a function of preheat temperatures. Here again the ore was allowed to cool to about 225°F before separation. It should be noted that efficiency of separation increases continuously with increasing preheat temperatures until incipient fusion of the ore takes place at about 950°F. The increase in optimum preheat temperature for Carlsbad ores over the pure minerals can be traced to the effect of the clay slimes intimately associated with the mined potash. If the slimes associated with the ore are removed by washing with alcohol or other non-aqueous material, the necessity of preheating to the high temperature is removed. This temperature range has been proved critical within these limits during continuous pilot plant operation. Concentrate and tailings grade and optimum recovery also are functions of the temperature of the potash mineral particles during separation in the electric field. Fig. 4 presents data indicating that feed to the rougher pass should range between 150°F and 275°F for best results. It has been found by subsequent pilot plant work that these temperatures can be maintained in actual operation.

Jan 1, 1959

The State Mining Experiment Station, Missouri School of Mines and Metallurgy, Rolla, Mo Charles H. Fulton, Director of the School of Mines Martin H. Thornberry, Director of the Mining Experiment Station. From the State Mining Experiment Station are issued all the general and technical bulletins of the School of Mines The latest bulletin containing a complete list of publications will be sent upon application to the Director of the Station Residents of the state may obtain bulletins as issued without charge, or may ask to be placed on the mailing list. Nonresidents should write to the Director for further information concerning specific bulletins. From the long list of bulletins the following have been care¬fully selected as being most likely to interest the geologist and the mining engineer. Vol 8, No. 1 (1916), Bibliography of concentrating ores by flotation, by J Cunningham, vol 1, No 3 (1912), Some apparatus and methods for demonstrating rock drilling and the loading of drill holes in tunneling, by L E Young, vol 2, No 1 (1915), Comparative tests of piston drill bits, by C R Forbes and L M Cummings; vol 2, No 3 (1916), Cupellation losses in assaying, by H. T Mann and C. Y Clayton; vol 4, No 1 (1917), The hydrometallurgy and electrolytic precipitation of zinc, by F D. James; vol 4, No 2 (1917), The effect of additional agents in flotation, pt 1, by M. H. Thornberry and H T. Mann, vol 5, No 1 (1919), The carbonization of Missouri cannel coals, by H L. Dunlap, K. K. Kershner and V. X Smiley. Vol 5, No. 4 (1921), Coal mining methods in Missouri, by W W Weigel, vol 6, No 1 (1921), The problem of the St Peter sand¬stone, by C L Dake, 50 cents, vol 6, No. 2 (1922), Bibliography on the electrothermic metallurgy of zinc, by B M. O'Harra, vol 6, No. 4 (1923), Experiments on the distillation of zinc from complex zinc-lead-silver ores, by B M. O'Harra and E S. Wheeler, vol 7, No 3 (1924), Underground loading devices, by C. E. van Barneveld, 81; vol 7, No. 4 (1924), Briquetting of zinc ores, by B. M. O'Harra; vol. 8, No 2 (1925), A treatise of Missouri clays, by M. H. Thornberry.

Jan 1, 1933

By R. S. Dean

THE commercial production of electrolytic manganese on a small scale commenced in 1939. The writer made a short report on the progress of production and utilization in MINING AND METALLURGY for January 1941. Progress during the last two years, naturally, has been more rapid. In June 1940, Congressman (now Senator) Scrugham presented a proposal to Congress for an appropriation authorizing erection of a pilot plant for "the production of metallic manganese by electrolytic or other means." As a result of this, a pilot plant, having a capacity of a few hundred pounds per day was built at Boulder City, Nev. Subsequent appropriations permitted expansion of the plant to about a ton per day. Much has been learned in this plant about electrolytic manganese, and the product even in its small way has found war uses of considerable importance. Meanwhile, the Knoxville plant of the Electro Manganese Corporation, the sole commercial producer, was expanded to about 4 tons per day to supply needed material for the war program. Other proposals for commercial plants have not been favorably received by the War Production Board. The Bureau reported on one such proposal by the American Alloys and Chemical Corporation. PRACTICE AT BOULDER CITY The present practice, as carried out at Boulder City, which is being described in more detail in a current paper by the Bureau staff at Boulder City, starts with a manganese dioxide ore containing about 20 per cent manganese. Currently this ore comes from the Three Kids deposit near Las Vegas. The steps for the production of electrolytic manganese, in general, are as follows: I. The manganese in the ore is reduced to MnO. 2. The MnO is dissolved from the ore in spent electrolyte, which contains about 38 to 47 grams per liter of free sulphuric acid, 135 grams per liter of ammonium sulphate, and 10 to 12 grams per liter of Mn as sulphate. In the leaching step the manganese is built back up to 32 to 36 grams per liter of Mn as sulphate; the pH is adjusted to neutral by means of gaseous ammonia and passed through thickeners. 3. The electrolyte is purified by adding H2S, which precipitates the heavy metals. After filtering, ferrous sulphate is added to the solution and oxidized with air and the solution is filtered and clarified on a precoat filter. 4. The purified catholyte is electrolyzed in a diaphragm cell using stainless-steel cathodes and lead-silver anodes. The current density is about 45 amp. per sq. ft. Current efficiencies of 60 to 65 per cent are regularly obtained.

Jan 1, 1944

By G. H. Kesler, C. E. Dryden, J. H. Oxley

Rates of heat- and mass-transfer from rods to recirculating air were determined within a one-quarter-scale model of a metals deposition bulb. The dependence of local and averaged rates of transfer upon outlet geometry, number of rods, position upon a rod, and airflow rate was established for flow patterns created by radial and tangential air inlets. The results are given a qualitative interpretation in terms of rates and distribution of metal deposition in a prototype deposition bulb. IT is well known that a number of metals can be prepared from volatile compounds containing them by causing dissociation of their compounds to occur at heated surfaces. Examples of such metals include silicon, titanium, zirconium, and aluminum, which can be prepared from their halides. While the ability to prepare high-purity metals by this technique is of importance in itself, the rate of deposition of metal also is important in considering the commercial potential of such a process. If the over-all process of deposition is broken down into separate steps of transport of materials to and from the heated deposition surface and establishment of chemical equilibrium at the surface, as was described in a recent paper,1 then since surface temperatures are usually high and surface equilibrium is attained very rapidly, the rate-controlling step can be considered as either that of transport of reactants to the surface or of transport of products other than deposited metal away from the surface. These two transport steps are related through the reaction stoichiometry. It can be shown1 that the rate and distribution of metal in such a transport-controlled process are determined by the over-all and local mass-transfer coefficients in conjunction with the equilibrium conversions at the hot surfaces. The rate relationship is: w = [KA(y a-y s)] B.E where the bracketed group is the rate of arrival of the reactant at the surface of area A as determined by the mole fraction driving force (y a - y s) and the convective transport constant K. The factor B is the weight fraction of metal in the reactant, and E is the equilibrium fractional conversion to metal. Numerical values of y, and y, are fixed by the vapor composition and the equilibrium compositim of reactant at the surface; and E can be determined by thermodynamic calculations or by experiment. However, values for the convective coefficient K are available generally only for systems of simple geometry, such as cross-flow past a rod or sphere or parallel flow past a flat plate or through a tube. Often it is necessary to work with systems of more complex geometry and in which the vapor flow may not be uniform or exactly parallel or perpendicular to the surface. It is possible, of course, to establish working correlations for these more complex systems by direct experiment; but the experiments usually are costly in both time and money. To circumvent this objection and to aid in arriving at an understanding of the relationships and interactions of the process variables, it is helpful to construct a model of the flow system in which air, water, or other convenient fluids can be substituted for the process vapors and with which mass-transfer measurements or analogous he at-transfer measurements can be made upon a simulated deposition surface. By this means, a large number of measurements can be made in a reasonable time, and the correlation of these results can be applied to the prototype system. Examples of the application of these techniques are to be found in the literature (e.g., Ref. 2). It is the purpose of this paper to illustrate these techniques by description of a model study which was done at Battelle Memorial Institute. The work to be described was of a preliminary nature; the investigation subsequently was extended to develop quantitative relationships among the significant dimensionless transport, geometric, and flow parameters. This more detailed study will be the subject of a future paper.

Jan 1, 1962

By R. Van A. Mills

ONE of the most important problems facing the petroleum industry is the profitable recovery of oil that is left underground by the ordinary methods of production. It is true that vast quantities of oil are being recovered from fields previously considered depleted by the pressure restoration method, the most widely applicable -and most successful means of obtaining greater recoveries that has thus far been, developed. But notwithstanding the progress that is being made in the field applica¬tion of this method there is urgent need for a better understanding of the fundamental principles that are involved. To meet this need the Petro¬leum Experiment Station of the U. S. Bureau of Mines at Bartlesville, Okla., during the past two years has conducted a series of intensive laboratory and field investigations. The larger part of the work has been carried on in the laboratory to supply the much needed information upon fundamental principles, information which few if any of the oil companies are in a position to supply for themselves. In all of this work the Bureau is endeavoring to correlate the results of laboratory investigations with those in the field, using the results of one to guide or check the other. This paper is primarily a progress report, briefly outlining the Bureau's methods of study, the laboratory and equipment in use, the preliminary problems that had to be solved in order to attack the major problems at hand, the methods of attacking some of the major problems, and some of the results of the investigations to date.

Jan 1, 1928

By J. Rogers, H. F. A. Hergt, K. L. Sutherland

IN 1938 Ralston4 reviewed the many attempts to find a satisfactory collector for the separation of cassiterite from its ores and in 1944 Dean and Ambrose2 summarized some further attempts. Generally, soaps and amines are effective but nonselective collectors. We have discovered that reagents containing either the polar group -SO4- or _S03- are excellent collectors for cassiterite and promise to be selective.1 The response to these reagents of cassiterite and of minerals commonly associated with it was studied, using the captive-bubble technique. Using these fundamental data, the practicability of separation and concentration of tin was investigated by flotation tests in a 2000gram Denver cell. EXPERIMENTAL METHODS Reagents All inorganic reagents were of Analar grade. The preparation and purification of sodium cetyl sulphate, cetyl trimethyl-ammonium bromide, laurylamine and cetylamine have been previously described.5 The other collectors were commercial surface-active agents, which were used without purification. Tests Captive-bubble Tests and Cylinder Flotation Tests have been previously described.5-10 The full lines shown in the figures relating solution composition to contact (flotation) distinguish solutions in which contact (flotation) is possible from those in which it is not. The curve is derived by successive approximation and the accuracy is ±0.2 pH units and ± 5 mg. per liter of collector or depressant. Solution compositions for which it was shown experimentally that contact or flotation is possible are marked by a circle, those for which it is not possible, by a cross, and those for which it is doubtful by a cross within a circle. It is assumed that at all other solution compositions within (without) the curve, contact or flotation is possible (not possible). After testing in the collector solution, the mineral was removed, washed, and tested by the captive-bubble method in water, or floated in a cylinder with frother only. In this way the composition of solutions in which a mineral was conditioned but in which properties of the collector solution prevented contact or flotation can be defined. The composition of solutions in which conditioning was possible lie between the full and broken curve, and the experimental results are indicated by a square. The curves show the limits of composition of solutions in which flotation in a cell would be possible but many factors other than those considered in these tests determine recovery and grade of a given mineral in practice. Flotation Tests in 500 and 2000-gram Denver Submachines.--Melbourne tap water, containing 12 parts calcium, 6 parts

Jan 1, 1947