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By L. E. Tanner

A study was made of the transformation kinetics of the commercial titanium-base alloys, Ti-2.5Al-16V and Ti-4A1-3Mo-1V, using two different heat treatment cycles: 1) step-quenching to aging temperatures from a ß solution anneal and 2) water-quenching from an a+ß solution anneal followed by reheating to aging temperatures. Metallographic examination and hardness testing provided the major portion of the data, while electrical resistivity, dynamic elastic modulus, and X-ray diffraction techniques were also used to obtain critical or confirnzatory data. TTT diagrams were constructed from these results. The sheet alloys, Ti-2.5Al-16V and Ti-4Al-3Mo-lV, are of current interest to the Department of Defense. As an aid to the planning of their respective heat treatments, a program was carried out to determine the transformation kinetics of these alloys using ß and a + ß reference states. This paper presents the TTT diagrams constructed from data obtained by metallographic examination and hardness testing, as well as by X-ray diffraction, electrical resistivity, and dynamic elastic modulus determinations. EXPERIMENTAL PROCEDURE Materials—Sheets of the alloys were obtained from the producers in the "mill anneal'' condition and were tested prior to shipment to assure their meeting mill specifications. Chemical analyses were also supplied and are presented in Table I. Heat Treatment—The majority of the data presented in this study were obtained from hardness testing and metallographic examination. Sample coupons were cut from the alloy sheets and heat treated on a mass scale. The annealing cycles were operated in the following manner: 1) The ß solution anneals were carried out in a horizontal tube furnace with the bare samples protected by a dynamic helium atmosphere. Following this treatment, the samples were quickly transferred to lead, solder, or oil-bath furnaces for aging. After prescribed times at the various reaction temperatures they were water-quenched. 2) The second cycle simulated commercial practice, which requires the alloys be quenched to room temperature following the a + ß sotution anneal. This anneal was carried out in a muffle furnace with a dynamic helium atmosphere. The specimens were then reheated from room temperature to the reaction temperatures in lead, solder, or oil-bath furnaces, followed by water-quenching after prescribed times at these temperatures. Information concerning the critical temperatures of the alloys was obtained from the literature and solution treatments were based on these values. A summary of the solution annealing treatments is found in Tables II and 111. The aging temperatures for the (a - ß alloys ranged in 50°C intervals from 200°C (392oF) to approximately 50°C below the ß/a + ß transus in the first cycle and approximately 50°C below the a + ß solution temperature in the second. The transformations in these alloys were known to be rather rapid, and thus aging times started at 0.5 min and went to a maximum of 7000 min. Hardness Testing and Metallographic Preparation— Heat-treated samples were sheared and mounted in Bakelite with their cut edges exposed. After a flat surface was ground, the hardness was determined in Vpn on an Armstrong-Vickers machine utilizing a 20-kg load. Three to four impressions were made on each specimen. After this procedure, the hardness impressions were removed and the edge surfaces of the specimens were prepared for metallographic examination in the usual manner. The etchant was 20 pct HF and 20 pct HNO3 in glycerine. Electrical Resistivity—It has been shown that the isothermal reactions in titanium-base alloys can be followed by measuring the changes in e1etrical resistivity attending these transformations. As mentioned earlier, the reaction kinetics of a-ß alloys are rather rapid; thus, it would be expected that resistivity data obtained from these alloys would be more significant if measurements were made continuously at the respective aging temperatures. To accomplish this end a special apparatus, based on the current-potential principle, was assembled. Its design was derived from earlier devices constructed by Colner and zmeska1 4 and Levinson.5 The set-up provided for the heat treatment zof machined specimens (approximately 2 x l0-4in. in cross section by 3 in. in length) and the determination of their relative

Jan 1, 1962

By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By S. G. Proctor, D. L. Baaso, W. V. Conner

A double crucible system was developed for I-g scale plutonium reductions. The equipment consists of an inner MgO crucible, an outer MgO crucible, and a stainless steel pressure vessel. The reduction charge is PIaced in the inner crucible and the annulus between the inner and outer crucibles is filled with a mixture of calcium and iodine. The exothermic reaction between the calcium and iodine in the annulus supplies the heat required for complete reaction of the reduction charge ana' good metal coalescence. Metal yields of 80 to 85 ,pct were obtained from I-g scale reductions and yields as high as 97.5 pct were obtained from 0.5-g scale reductions. The system was used to reduce charges containing as little as 0.1 g of Pu resulting in metal yields up to 90 Pct. THIN metal foils of highly enriched plutonium isotopes are used as targets for cross section and other measurements. The isotopes are separated in the calutrons at Oak Ridge and are very expensive to prepare. Often, only 1 or 2 g of material are available thereby emphasizing the need for a method of preparing these small quantities of metal. Procedures for 1-g scale plutonium reductions have been described, but these procedures require elaborate or expensive equipment. For example, the procedure described by Anselin et al.1 requires an inert atmosphere glovebox and induction heating equipment. The procedure described by Baker2 also uses induction heating equipment to obtain the recommended heating rates and liner temperatures. Baker's procedure also requires high purity PuF4 with very little PuO2 present. The procedure described in this paper resulted from a search for a simple and inexpensive method for making 1-g scale plutonium reductions. EXPERIMENTAL Equipment. The equipment required for the double crucible system consists of a pressure vessel, two MgO crucibles, a MgO crucible lid, and a resistance-heated, vertical crucible furnace. The crucibles were slip cast from high purity MgO and were supplied by the Coors Porcelain Co. and the Norton Co. The pressure vessel and lid were fabricated from 316 stainless steel. Materials. The PuF4 used for this study was obtained from the P1utoniu:m Metal Production Department at Rocky Flats. The PuF4 was prepared in a con- tinuous hydrofluorinator by reacting Pu02 with HF at 650°C. The isotopic composition of the plutonium was approximately 93 pct 239PU, 6 pct 240PU, and 0.5 pct 241PU. Some of this PuF, contained less than 1 pct Pu02 (Batch No. 6 and 7), while other batches contained up to 15 pct Pu02 (Batch No. 3). The chemical analyses of all the PuF4 used for this study is given in Table I. The calcium was 99 pct pure, AEC grade, and only that fraction which would pass through a 20 mesh screen was used. The I2 was USP grade re-sublimed I2 which was ground before being used. Procedure. Various charge compositions and methods for loading the double crucible system were tested. The optimum conditions for 1-g scale reductions are described below. The double crucible system was loaded as shown in Fig. 1. The outer crucible was placed in the pressure vessel and the annulus between them was filled with MgO sand. The inner crucible was placed in the outer crucible, supported by a layer of MgO sand in the bottom of the outer crucible. A mixture of 5.2 g of Ca and 25 g of I2 was placed in the annulas between the two crucibles. The upper portion of the annulas was filled with MgO sand. Next, a layer of a mixture of calcium and I, equal to 20 wt pct of the calcium and I2 used in the main charge was placed in the bottom of the inner crucible. The PuF, to be reduced was mixed with a 30 pct excess of calcium and 1 mole of I2 per mole of Pu and this mixture was placed in the inner crucible. The charge was topped with a layer of a mixture of calcium and I2 equal to 20 wt pct of the calcium and I2 used in the main charge. The pressure vessel was sealed with a flat copper gasket and was purged by alternately evacuating and filling with argon. The purge valve was closed and the vessel was placed in a vertical crucible furnace which was preheated to 950°C. The furnace was turned off after 20 min of heating and the vessel allowed to cool. Experience has shown that. this amount of heating is sufficient to assure complete reaction of the charge. RESULTS AND DISCUSSION The double crucible system has been used to produce plutonium metal on a 0.1- to 1-g scale. Reduction

Jan 1, 1970

By P. Chiotti, G. R. Kilp

Thermal, metallographic, vapor pressure, and X-ray data were obtained to establish the phase diagram for the zinc-zzrconiz~m system. Five compounds corresponding to the stoi-chiometric formulas ZrZn, ZrZn,, ZrZn,, ZrZn,, and ZrZn14 were observed. All these compounds, with the exception of ZrZn2, which melts congruently at 1180°C under constrained zinc-vapor conditions, undergo pexitectic reactians. The temperature at which the zinc vapor pressure is I atm for a series of alloys was determined from vapor-pressure measurements. The data obtained are summarized in the construction of a I-atm-pressure phase diagram and a phase diagram corresponding to a pressure of less than 10 atm. THE purpose of this investigation was to establish the phase diagram for the zinc-zirconium system. Thermal, metallographic, vapor pressure, and X-ray data were employed in determining the phase regions. Partial investigations of this system have been conducted by Gebhardt1 and Carlson and Borders.' Carlson and Borders studied the high-zirconium region and established the existence of a eutectic at 69 wt pct Zr with a melting point of 1015°C. The terminal phases of the eutectic horizontal were shown to be an intermetallic compound ZrZn and a solid solution of ß zirconium containing 21 wt pct Zn. The ß solid solution decomposes into ZrZn and a zirconium at 750°C. The eutectoid composition is given as 15 wt pct Zn, and the solubility of zinc in a zirconium at temperatures below 750°C is indicated to be negligible. Gebhardt studied the zinc-rich region and observed a lowering of the melting point of zinc from 419.5" to 416°C and temperature horizontals at 545" and970°C. Some preliminary observations by Chiotti, Ratliff, and Kilp were reported by Hayes.2 pietrokowsky3 has reported the compound ZrZn2 to have a cubic MgCu2 structure with ao = 7.396A. MATERIALS AND EXPERIMENTAL PROCEDURES The metals employed in the preparation of alloys were Bunker Hill slab zinc or Baker analyzed reagent granulated zinc, both 99.99 pct pure and hafnium-free iodide-process crystal bar zirconium obtained from the Westinghouse Electric Corp. The zirconium contained 200 ppm Fe, 200 ppm Si, 100 ppm C, and minor amounts of other impurities. The zirconium was milled or machined into thin chips or shavings. These were cleaned with a nitric-hydrofluoric acid solution, rinsed with water, and acetone, and dried just prior to their use in alloy preparation. The granulated zinc was similarly cleaned using dilute nitric or hydrochloric acid. Weighed quantities of these materials, 20 to 30 g total, were mixed and pressed at 20,000 to 70,000 psi to give relatively dense compacts. During the early part of this investigation the pressed compacts were placed in MgO-15 wt pct MgF, crucibles which were then sealed inside of quartz ampules. The compacts were given various prolonged heat treatments prior to their use for thermal analyses, or vapor-pressure measurements. Because of expansion of the compacts and the relatively high zinc vapor pressure it was difficult to heat to the melting temperatures of the alloys without failure of the quartz ampules. Homogenization at temperatures below the melting temperature gave brittle, porous alloys unsuitable for metallographic examination. It was also difficult to prevent condensation and segregation of zinc on the colder parts of the quartz ampules during heating and cooling operations. These problems were eliminated to a great extent by the use of tantalum crucibles. Tantalum proved to be a satisfactory container with little or no reaction between the alloys and the tantalum. Small tantalum thermocouple wells were successfully welded in the bottom of these crucibles. Pressed compacts were sealed inside the tantalum crucibles by welding on preformed caps under an argon atmosphere. Heat treating and differential thermal analysis were combined into a single operation. The experimental sample assembly is shown in Fig. 1. This assembly was enclosed inside a stainless-steel tube heating chamber which could be evacuated and filled with an inert gas. The thermocouple leads were brought out of the heating chamber between two rubber gaskets used to provide a vacuum seal for the water-cooled head. Most of the compounds in this system undergo peritectic decomposition. After heating above the temperature of a particular peritectic horizontal the sample was cooled to just below the peritectic temperature and held at temperature for several hours. The sample was then reheated through the peritectic temperature and the size of the thermal arrest, if still present, compared with the one previously obtained. If the thermal arrest was not characteristic for the alloy composition being investigated its magnitude diminished and repeated cycling and annealing eventually eliminated it. The peritectic thermal arrests characteristic of a particular composition were established in this manner.

Jan 1, 1960

By L. C. Michels, O. G. Ricketts

The disorientations between s?nall grains, whose growth has been arrested at an early stage of recrys-tallization, and the deformed matrix in cold-rolled aluminum single crystals were determined using transmission Kikuchi line and electron diffraction patterns. The orientations of the recrystallized grains were found to be random, and the disorientations of these grains with the matrix weve found to be intermediate to large. This leads to the conclusion that the observed vecrystallization began in small areas of large disorientation present in the cold-worked structure. heavily cold-worked thin sections of aluminunz single crystals and of polycrystalline aluminum and nickel were produced directly by a mechanical technique. The specinlens thus prepared were heated with the electron beam to bring about vecrystallization during observation in the electron microscope. Motion pictures taken du.ring heating and the electvon, microg.raphs taken both before and aftev heating allowed the recrystallization process to be traced to its ovigin. Re cvystallized grains originated in very s,mall regions of the cold-worked structure and developed through rapid migration of high-angle boundaries. The boundaries either were present as such in the matrix or were formed out of dense dislocation networks. SIGNIFICANT advances have been made in recent years in the study of nucleation of recrystallization using the technique of transmission electron microscopy of thin metal foils. Bollman1 in a study of heavily rolled polycrystalline nickel found support for the Cahn-Cottrell2,3 theory of nucleation. According to this theory nuclei form by the initially slow growth of subgrains formed through polygonization. During this initial period of slow growth (the incubation period) the migrating boundary of the subgrain increases its disorientation with the cold-worked matrix and thereby increases its mobility to become a rapidly migrating high-angle boundary. Bailey4,5 investigated the annealing behavior of several metals deformed both in tension and by rolling and concluded that recrystallization took place through the migration of high-angle boundaries. With low deformations these boundaries were present in the metal before deformation. With high deformation it was not possible to tell whether the boundaries were pieces of the original grain boundaries or were produced either during deformation or by polygonization during ameal- ing. Direct observation during heating of metal foils indicated that subgrains form by polygonization and grow at an uneven rate. The grain size obtained decreased with decreasing foil thickness indicating that the foil surface resists boundary motion. Votava,6 in heating stage experiments on rolled copper, observed nuclei to appear suddenly and grow in jumps of differing magnitude. However, he found no special dislocation configurations where the nuclei appeared. Fujita,7 as a result of a study of subgrain growth in heavily worked aluminum, concluded that the boundary of a recrystallized grain initially forms from the boundary of a group of subgrains. This occurred by a process of deposition of vacancies and dislocations in the group boundary as the boundaries within the group disappear. HU8,9 directly observed a similar process in heating stage experiments on 70 pct rolled Si-Fe single crystals. The growth of subgrains appeared to proceed by a coalescence mechanism. The observed fading away of the boundary between two subgrains was explained by the moving out of dislocations from the disappearing boundary into the connecting or intersecting boundaries around the subgrains. The subgrain size and degree of disorientation with the surrounding structure were thus increased. With the increase in disorientation occurred a corresponding increase in boundary mobility, which eventually allowed the boundary to migrate rapidly. This process was observed to occur within "microbands" consisting of parallel narrow segments disoriented by a few degrees present in the as-rolled structure. The conclusion of Rzepski and Montuelle10 that growth is preceded by the coalescence of blocks through disappearance of their common boundaries supports this view. In contrast to Hu's coalescence model for nucleation were the conclusions of Walter and ~och.""~ Working with the same material as Hu, of the same orientation and rolled to the same reduction, they concluded that nucleation occurred by the Cahn-Cottrell mechanism. They observed, in agreement with Hu, that recrystallization began in the "microband" regions which they referred to as "transition" bands. Bartuska13 studied subgrain growth in heavily rolled nickel using a beam heating method in the electron microscope. He concluded that nuclei for recrystallization form from the largest most perfect subgrains present in the cold-worked structure by rapid intermittent migration of parts of subboundaries. In rare instances he observed subgrain growth by coalescence. EXPERIMENTAL PROCEDURE The materials used in this study were 99.999 pct A1 supplied by A.I.A.G. Metals, Inc., and 99.999 pct Ni supplied by Johnson and Matthey and Co., Ltd. The Hitachi HU-11 electron microscope, with uniaxial

Jan 1, 1968

By AIME AIME

Do you Possess, or Can you Obtain; and Will you Give, or Sell, to the Institute Library Early Volumes of the following Proceedings and Journals? American Chemical Society. American Foundrymen's Association. Australian Mining Standard. Chemical Society of London. Deutsche Chemische Gesellschaft. The Foundry. New Zealand Mines Record. Queensland Government Mining Journal. La Revue Universelle des Mines.

Jan 9, 1907

By David Mandolesi

An examination has been made of the structures of strand cast blooms and the rails rolled from them; this paper details the characteristics of these typical structures. Results of mechanical testing data show that this product compares with rails processed from conventional ingot steel. Improvement in processing yields and surface quality standards are also briefly discussed.

Jan 1, 1972

By D. S. Jacobus

The boiler here referred to was of the water-tube type, having 2535 square feet of heating-surface, which the makers held to be capable of generating 325 horse-power of steam; this being understood to mean that 325 times 30 pounds of water would be evap-

Jan 1, 1889

By Edgar Rickard

E UGAR RICKARD comes of a long line of mining men and was born at Pontgibaud, France, in 1874, where his father was then in the course of his professional work. Later his father came to California and was until his death prominently connected with milling in that state and Nevada. Edgar Rickard grew up at Berkeley, attended the University of California, graduated in 1895 from the mechanical engineering course, and remained a year longer for post-graduate work in the College of Mining. His first job was as assarer for the Mountain Copper Co., Keswick, Cal., in 1896. The following year he was assayer and surveyor for the Cornucopia Mines, Oregon. In 1898, he joined the staff of the Venture Corporation, London, and for two years made examinations for them in various parts of the world. He served as mine manager at Cripple Creek and at the Briseis tin mine, in Tasmania. From 1901 to 1905, he was general manager of the Progress Mining Co. in Lower California, but when his cousin, T. A. Rickard, bought the Mining and Scientific Press he was persuaded to come to San Francisco as business manager of that periodical. A few years later the two cousins went to London and started the Mining Magewine there as a joint venture, Edgar being the business manager. In 1915, he took over control, T. A. Rickard returning to California to devote his time to the Mining u.rbd Scientific Press. In 1917 Edgar Rickard sold out to his British associates and came home to serve in the Food Administration through the war. Rickard was one of the first of the American engineers called to his staff when Herbert Hoover began his relief work by helping stranded Americans home at the be- ginning of the war and he has been with him constantly since in the Commission for Relief in Belgium, the

Jan 1, 1929

By W. C. Knopf, G. Samsel

For several years International Minerals & Chem-ical Corp. has used a radiation method to assay potassium content of products from potash and feldspar beneficiation. The procedure is rapid, accurate, and inexpensive and is easily handled, if necessary, by nontechnical personnel. Data are presented to show the accuracies that may be expected if the technique is used for control of pilot plants or large-scale plants. Natural potassium is composed of three isotopes —K, K and K. Five other isotopes, artificially produced, have been detected. In natural potassium only the K isotope, with a half life of 1.4x10 years, is radioactive. Its modes of decay are beta and gamma rays, positrons, and x-rays. Only the more abundant beta rays, however, are important in radiation measurements using geiger tubes. Barnes and Salley' measured radiation of potassium salts in solution in 1943. Gaudin and Parnell2 first reported the use of solid salts arranged in a vessel surrounding the ß counter in 1948. Later, Scheel used the method to assay potassium content of various crude and finished potash salts. Experimental: Dip-type Geiger-Muller tubes (TGC-5) supplied by Tracerlab Co. were used in all radiation counting measurements. The tube was encompassed by a glass container about M in. larger in diameter than the tube. This container, which served as a sample holder, was closed at the bottom with a rubber stopper to facilitate removing the samples. Samples were not weighed, but about 40 g of sample were needed for each test. Electrical impulses from the tube were counted on either a Tracerlab scaler or a rate meter. To obviate the need for constant attendance, preset features were incorporated into the scalers, so that at a predetermined time or count the units were automatically deactivated. When rate meters were used, counting rates were read directly from instrument or from a recorder used in conjunction with the rate meter. Each tube was calibrated, according to the manufacturer's instructions, to determine the correct operating voltage to insure reproducible results. A linear calibration plot of percent K2O vs counting rate was also obtained for each tube by recording the counting rate plus background count of several standards of different K2O content chemically analyzed by the chloroplatinate method.' These standards were of approximately the same particle size distribution as samples to be assayed. Specific background count caused by cosmic rays and other surrounding radiation was checked periodically by counting a sample of pure NaCl. Fig. 1 is a representative calibration plot. Assays were determined directly from the standard plot or calculated by subtracting the background count from the counting rate, then multiplying by the slope of the line. Chemical assays of the test samples were made by the Sherril method," a flame photometric technique, or the chloroplatinate method. Data: The radiation assay method has been used for three years by International Minerals & Chemical Corp. in the laboratory and in pilot plants processing ores containing potassium. These dry concentration plants process sylvinite and langbeinite ores at Carlsbad, N. M., and feldspar ores at Top-sham, Maine. Sylvinite ore is predominantly a mixture of syl-vite (impure KCl) and halite (impure NaCl). Contaminants include sulfates, such as langbeinite (2MgSO - K2SO4), kieserite (MgSO H2O), poly-halite (MgSO4.K2SO, 2CaSO, . 2H2O), and slimes. Langbeinite ore is predominantly langbeinite and halite with small amounts of sylvite, sulfates other than langbeinite, and slimes. Several variables, in addition to correct calibration and standardization of tubes, were found to be important in obtaining reproducible results. Particle size distribution of standard samples should be

Jan 1, 1959

By M. R. Geer, H. F. Yancey

THE performance of coal-washing equipment, that is, the effectiveness with which coal and impurity are separated, is a subject of undisputed interest to all concerned with the preparation of coal. Through the years much has been written in both American and European literature on the performance of coal-washing equipment and its interpretation, but until recently no effort has been made to consolidate this wealth of information into a single, comprehensive treatment of the subject. A splendid effort in this direction was made at the First International Conference on Coal Preparation held in Paris in June 1950 in which representatives from virtually every coal-producing country participated. Although the scope of the conference covered the entire field of coal preparation, many of the sixty-odd papers and a great deal of the discussion dealt with the subject of evaluating washery performance. Prominence was given this subject by the Centre d'Etudes et Re-cherches, des Charbonnages de France, which sponsored the conference. This research organization, generally referred to as Cerchar, was formed in 1948 following the nationalization of the French coal industry. Since that date it has conducted an intensive study of coal preparation. Perhaps because of a fresh viewpoint, Cerchar realized immediately that complete information on the performance of French washeries and a thorough understanding of the mechanism of gravity separation were the fundamental prerequisites in a program to improve preparation practice. For this reason Cerchar concentrated on obtaining performance data and on a comprehensive study of methods of evaluating such information. Some idea of the magnitude of this work will be appreciated from the fact that 175 performance tests were made in 44 plants. The work performed by Cerchar emphasized a condition that is recognized by many of those concerned with coal preparation, namely that the lack of uniformity in presenting data on washery performance, the diversity of methods used in evaluating such information, and the frequent confusion of the terms related to performance have been prime factors militating against the progress from art to science. Thus, Cerchar feels that standardization of the methods employed for evaluating washery performance, not only in France but in the entire world, is essential to progress, and the prime objective of the Paris conference was to seek international standardization of the evaluation methods advocated by Cerchar. At the conclusion of the conference the question of standardization was referred to the International Standards Organization. A careful study of the dozen papers on the subject of evaluating washery performance presented at the conference reveals that none of the methods is new; most of them date back over a decade. Nevertheless, the intensive scrutiny of these methods brought about by the conference unquestionably has resulted in a valuable exchange of ideas and a clarification of thought that could scarcely be achieved in any other way. The object of the present report is to make available to the American coal industry the ideas developed at the conference which seem most important from an American viewpoint and to provide a critical analysis of some of the evaluation methods advocated by Cerchar. The various methods of evaluating washery performance are illustrated partly with data that have been published in American literature, and some new data have been obtained as the result of experimental work undertaken since the conference to provide information on certain controversial points. An English translation of the proceedings of the conference, including the discussion as well as the papers, will be available,' and previous to the conference Coal Age2 published a very brief description of some of the principal evaluation methods used by Cerchar. Americans will appreciate as well as do the French the desirability of standardizing both the termi-

Jan 1, 1952

By H. R. Hanley

The characteristics of alloyed anodes and their influence on the products of electrolysis and power consumption have been noted previosly ously in the literature.' This paper presents data in continuation of the subject given in an earlier paper by the authors.2 As noted in the authors1 previous paper, the objectives of this work are the reduction in the cell voltage and the purity of the cathode product resulting from the use of alloyed lead anodes. The fundamental facts developed in the previous paper were: (I) that the presence of a small amount of calcium lowers the anode potential approximately 50 per cent. below that of pure lead; and (2) that thallium when present to the extent of 4 per cent. rendered the anode practically stable, thereby lowering the contamination of the cathode by lead to a very insignificant amount. The specific features determined in this recent work are as follows: 1. The lowest limit of calcium in the lead which will still give maximum lowering of the anode potential. 2. The characteristics of the thallium-calcium-lead anode. 3. The characteristics of the silver-calcium-lead anode. 4. The characteristics of the thallium-silver-calciurn-lead anode. It was determined that 0.1 per cent. calcium in the anode was sufficient to lower the anode potential approximately 50 per cent. Table 1 shows the characteristics of alloyed anodes tested. The anode composed of 0.1 per cent. calcium, 4 per cent. thallium, and 95.9 per cent. * Professor of Metsllurgy, Missouri School of Mines. t Professor of Metallurgy and Ore Dressing, Hea.d of Department, Missouri School of Mines. Assistant Professor of Metallurgy, Missouri School of Mines. 1 Among others, see C. G. Fink and Li Chi Pan: Insoluble .Anodes for the Electrol-ysis of Brine [Trans. Amer. Electrochem. Soc., (1926) 49, 83-1341 and other papers by these authors. U. CJ. Taintori, 8. G. Taylor arid H. P. Ehrlinger: Lead Alloys for Anodes in Electrolytic Production of Zinc of High Purity. Truns. A. I. M. E. (1929) 192-200. 2 H. R. Hanley, C. Y. Clayton, D. F. Walsh: Investigation of Anodes for Production of Electrolytic Zinc. Trans. A. I. M. E. (1930) 275

Jan 1, 1931

By Roy E. Dickerson, W. M. O Connor

The production of crude petroleum of the Bacuranao field, Cuba, fell off rapidly because no new wells Mere drilled. In December 1938, the total was 15 bbl. per day. The estimated average from this serpentine field for the year is 20 bbl. per day. The Motembo area produced an estimated average of 160 bbl. per day. Production in July was 215,946 gal of gasoline, or 165 bbl. per day. In August production was higher because a new well in the concession, the Luisa Marcela, produced 189 drums the first day and required pit storage. The Atlantic Refining Company of Cuba started a deep test upon a long, narrow, surface-defined anticline 3 km. south of Remedios, a town on the north coastal plain of Santa Clara province, in December 1938. The Atlantic Refining Co. is doing extensive seismograph arid gravity-meter work in Matanzas arid Santa Clara provinces. The Shell company was rigging for a deep test in western Havana province at a location about 2 km. west of the town San Antonio dc los Banos New Petroleum Law More serious attention was given by some of the major oil companies to the development of petroleum in Cuba as a, result of the passage of a Petroleum Law ill that country on May 9, 1938. Under the old mining lam of Cuba, which gave no special treatment to petroleum, the usual provisions giving reasonably satisfartory guarantees to encourage investmerit of foreign capital were either entirely lacking or were 30 ambiguously expressed as to require legislative action. Under the new law, Government royalty is fixed at 10 per cent with the provision that it will be reduced to 9 per cent on crude petroleum that is refined in Cuba. Royalty to the surface owner is 1 per cent. A surface tax on a sliding scale from 10¢ to 406 per hectare per year is applicable to all exploitation concessions granted under the law or adapted to its provisions. So export tax is payable upon petroleum. Stability of taxation

Jan 1, 1939

By Joseph C. Buchen

In principle, productiorl of salt from sea water is a simple operation. The sun and wind cause evaporation of sea water trapped in ponds, and what is left is principally salt. Commercial production, however, requires consideration of many factors. First is a high consistent annual rate of evaporation, as well as large areas of suitable low-lying ground close to economical shipping facilities. The south end of San Francisco Bay has these requisites. Large ponds are built, by using clamshell dredges to build up levees to a height of approximately 3 ft. on ground usually lower than sea level, so that the water may be taken in through tide gates without pumping. Ponds are divided into extremely large concentrating ponds and smeller crystallizing ponds. Approximately ten times more area is required for concentrating than for crystallizing. The concentrating ponds are irregular in shape and size but the crystallizing ponds are rectangular and fairly regular in size, to aid in harvesting. The ocean water is taken into the first of a series of concentrating ponds and gradually moved forward from pond to pond as it increase:: in density, reaehing the crystallizing area as a saturated brine. This brine is pumped into the crystallizer at the beginning of the net evaporating season, usually in May, and further evaporation causes its sodium chloride content to deposit on the bottoms of the ponds. The brine must be drawn off and a fresh supply added from time to time to prevent other undesirable salts from depositing with the sodium chloride. Harvesting usually begins near the end of August and now is accomplished almost entirely by mechanical means. After harvesting, the salt is stored in large sbockpiles until required for shipping or refining. The greatest amount is used for industrial purposes and is shipped without any processing other than screening, but all salt for domestic use produced by the Leslie Salt Co. is refined by the racuum process, giving a produet consistently testing over 09.9 per cent sodium chloride.

Jan 1, 1938

By Joseph C. Buchen

In principle, productiorl of salt from sea water is a simple operation. The sun and wind cause evaporation of sea water trapped in ponds, and what is left is principally salt. Commercial production, however, requires consideration of many factors. First is a high consistent annual rate of evaporation, as well as large areas of suitable low-lying ground close to economical shipping facilities. The south end of San Francisco Bay has these requisites. Large ponds are built, by using clamshell dredges to build up levees to a height of approximately 3 ft. on ground usually lower than sea level, so that the water may be taken in through tide gates without pumping. Ponds are divided into extremely large concentrating ponds and smeller crystallizing ponds. Approximately ten times more area is required for concentrating than for crystallizing. The concentrating ponds are irregular in shape and size but the crystallizing ponds are rectangular and fairly regular in size, to aid in harvesting. The ocean water is taken into the first of a series of concentrating ponds and gradually moved forward from pond to pond as it increase:: in density, reaehing the crystallizing area as a saturated brine. This brine is pumped into the crystallizer at the beginning of the net evaporating season, usually in May, and further evaporation causes its sodium chloride content to deposit on the bottoms of the ponds. The brine must be drawn off and a fresh supply added from time to time to prevent other undesirable salts from depositing with the sodium chloride. Harvesting usually begins near the end of August and now is accomplished almost entirely by mechanical means. After harvesting, the salt is stored in large sbockpiles until required for shipping or refining. The greatest amount is used for industrial purposes and is shipped without any processing other than screening, but all salt for domestic use produced by the Leslie Salt Co. is refined by the racuum process, giving a produet consistently testing over 09.9 per cent sodium chloride.

Jan 1, 1938

By C. L. Dake

Discussion of the paper of. C. L. DAKE, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 103, July, 1915, pp. 1429 to 1436. A. C. LAWSON, Berkeley, Cal.-It appears that our bog-iron ores are due in a large measure to the activity of certain iron bacteria, and a paper dealing with this subject that makes no reference to that particular agency strikes me as rather curious. C. L. DANE, Rolla, Mo.-Mr. Lawson's criticism that this paper makes no reference to the activity, of iron bacteria is scarcely true. On p. 1430 I stated: "Certain bacteria precipitate iron by building the hydrated oxide into their body cells," and again, "There are many other means by which, under special conditions, iron may be precipitated in nature. Oxidation, evaporation of CO2, and iron bacteria have been held to be the most important." Thus the activity of bacteria receives as extended mention as the action of any other agency in precipitation of iron. The paper makes no pretense of covering exhaustively the origin of bog ores, but, as its original title suggested, refers to Some Principles Controlling the Formation and Distribution of Bog Iron Ores. Mr. Lawson seems to have entirely missed the main thesis of the paper, which attempts to establish some relation between glaciation and abundance of bog ores now forming. Unfortunately, I have no immediate access to the literature of the subject, but my best recollection is that the data regarding iron bacteria throw no light whatever on the cause of bog ores being so much in ore abundant within the limits of the glaciated regions, and being reported much less frequently from the tropics. This lack of data is suggested in the following (p. 1434): "It has already been shown that bacteria aid in the precipitation of iron. Whether tropical conditions increase or decrease the activity of such bacteria is unknown."

Jan 12, 1915

By Robert Livermore

THE Smuggler-Union mine is in the upper San Miguel mining district near Telluride, Colo., and the group of claims now forming the property were first worked in 1875. Development was slow until the completion of the railroad in 1890, when it pro- ceeded rapidly. In 1896 four hundred stamps were dropping in the district, the production was $3,000,000. A geologic section of the country rocks, where ex-posed by erosion from the valley at 8700 ft. to the sum-mit at 13,500 ft., shows the sedimentaries made up of flat-bedded sandstones and conglomerates, of the Jura-Trias, superimposed at 9700 ft. by a series of bedded rocks of igneous origin, andesites and andesite breccia. These rocks extend 3000 ft. to the rhyolite capping, largely fragmentary, which occurs at 13,000 ft. The ore horizon is, so far as known, contained in the 3000 ft. of' andesite and breccia. The Smuggler vein is a fault fissure which, with its extension to the north, the Humboldt vein, contains one of the longest continuously mined orebodies in the world. The length of the orebody so far developed is approximately 9000 ft. The width of the valuable part of the vein is, however, narrow, 3 ft. being the average, and the depth to which it has been worked up to the present is 2500 feet. There are several crossing and branch veins, all of which have been more or less productive. Of these, the so-called Flat vein, discovered in 1915, with its pro-duction of nearly 2,000,000 tons, has been the most important. This vein joins the Smuggler at an acute angle in the northern section of the property. North of the junction the two veins lie side by side and form an orebody of importance which gives promise of exten-sion with depth. The valuable metals of both the Smug-gler and Flat veins are gold, lead and silver. In the former silver is more important than lead, and the reverse relation holds in the latter.

Jan 3, 1928

By W. M. O Connor, Roy E. Dickerson

The production of crude petroleum of the Bacuranao field, Cuba, fell off rapidly because no new wells Mere drilled. In December 1938, the total was 15 bbl. per day. The estimated average from this serpentine field for the year is 20 bbl. per day. The Motembo area produced an estimated average of 160 bbl. per day. Production in July was 215,946 gal of gasoline, or 165 bbl. per day. In August production was higher because a new well in the concession, the Luisa Marcela, produced 189 drums the first day and required pit storage. The Atlantic Refining Company of Cuba started a deep test upon a long, narrow, surface-defined anticline 3 km. south of Remedios, a town on the north coastal plain of Santa Clara province, in December 1938. The Atlantic Refining Co. is doing extensive seismograph arid gravity-meter work in Matanzas arid Santa Clara provinces. The Shell company was rigging for a deep test in western Havana province at a location about 2 km. west of the town San Antonio dc los Banos New Petroleum Law More serious attention was given by some of the major oil companies to the development of petroleum in Cuba as a, result of the passage of a Petroleum Law ill that country on May 9, 1938. Under the old mining lam of Cuba, which gave no special treatment to petroleum, the usual provisions giving reasonably satisfartory guarantees to encourage investmerit of foreign capital were either entirely lacking or were 30 ambiguously expressed as to require legislative action. Under the new law, Government royalty is fixed at 10 per cent with the provision that it will be reduced to 9 per cent on crude petroleum that is refined in Cuba. Royalty to the surface owner is 1 per cent. A surface tax on a sliding scale from 10¢ to 406 per hectare per year is applicable to all exploitation concessions granted under the law or adapted to its provisions. So export tax is payable upon petroleum. Stability of taxation

Jan 1, 1939

By E. T. Dumble

For many years there have been occasional reports of the discovery of gold from a belt of the coast country of Texas which is underlain by deposits belonging to the lower Eocene. For the most part they have been treated as newspaper reports and no examination or record of them has been made. Among such, it may be mentioned that in 1896 there was a flurry over reported gold-discoveries west of Luling and elsewhere in this belt, and in 1903 some prospect-shafts were sunk on the Gon-zales branch of the Galveston, Houston & San Antonio railway, 3 miles below Harwood. During 1912, further discoveries have again brought the matter to our attention, and it may be of interest to record the facts as we have found them. Some years ago specimens were sent me, which were said to have been taken from certain beds on Gazley creek, and concentrated by washing in a rocker. In them were several particles of gold sufficiently large to be visible to the eye. Under the microscope they showed to be, with few exceptions, sharp cornered, and not rounded as is usual with placer-gold. They were not filings, however, but their sharpness seemed rather to be due to a recent freeing from their matrix. One or two grains were rusty, and one copper-hued, but the most of them were tolerably bright. On examining the material of the samples small grains or fragments were found, of a yellowish brown color, which seemed to be of a finely-granular structure—possibly a sandstone. In these fragments I found particles of gold, one of them being large enough to be visible without a lens. Gazley creek empties into the Colorado river just north of Smithville, and for a few miles north of that place its banks show, beneath the deposits of more recent materials, the sands and clays of the Lignitie division of the Eocene, with lignite, shells of iron, etc.

Jan 1, 1913