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By J. J. Mulligan, F. F. Colcord, E. F. Kern

The electrolytic separation of silver and gold has been practiced by the refineries in the United States for a good many years, and probably because of frequent visiting between officials of plants and the consequent exchange of views, operations in the various silver and gold refineries are very similar. We find, for instance, they practically all use electrolytes of approximately the same composition, which, no doubt, is more the result of experience than of studies of electrolytes. At the new electrolytic parting plant of the U. S. S. Lead Refinery, Inc., East Chicago, Ind., considerable attention has been given to the composition of electrolytes, especially to their conductivity and their effect on the character of the silver deposit. We are not aware that anything has been recently published on this subject and are, therefore, presenting such data as we have with the idea that, although it will not be wholly new, it may stimulate interest in the subject. Effect of Copper Content on Conductivity The first work was to determine the specific conductivity of silver nitrate and copper nitrate solutions. Concentrated solutions of silver nitrate and copper nitrate were prepared by dissolving analyzed chemically-pure salts in distilled water, and determining the silver and copper in each. Definite amounts of the concentrated solutions were taken, mixed and diluted to a definite volume. The silver and the copper were determined in each of these solutions and the conductivity was then determined. The plotted results are shown in Figs. 1 and 2. The effect of increasing quantities of silver and copper is readily seen. A comparison of the two sets of curves shows conclusively the benefit of holding the copper content of the electrolyte above 5C g. per liter, as its effect is to increase greatly the conductivity in an approximate propor-

Jan 1, 1926

By E. A. Reilly, G. R. Gardner, F. P. Lasseter

THE methods that may be applied to the treatment of slurries and water, as these are related to practical coal-preparation problems, are concerned essentially with the movements of solids suspended in water. It is assumed that there are no fundamental differences between the principles involved in the treatment of coal slurries and the phenomena encountered in general mineral-dressing practice, and the latter are presented in some detail. Basic principles are correlated with present practice for both the anthracite and the bituminous coal. fields, and meth¬ods are discussed which are designed to utilize best all the material subjected to treatment and suggest a sound approach to the solution of problems relating to the return of clear water to process or to streams. In order to approach the practical phases of the subject with sufficient understanding of the basic principles, it is necessary to discuss two types of phenomena that are applicable. The first is flocculation and the second is sedimentation. Descriptive matter is given covering the various meth¬ods and types of equipment employed to conduct these operations, with emphasis on their application to water and coal-slurry treatment.

Jan 1, 1943

By O. D. Sherby, J. E. Dorn

For elevated temperature-constant load creep tests of a solid solution alloys, the creep strain is a function of a temperature-compensated time parameter 0 = je H/RT dt. The activation energy H is equal to o constant of about 36,000 cal per mol. The substructures resulting from a given creep stress condition are functions of the creep strain independent of temperature. Each new creep stress gives a new unique set of grain substructures; this is one of the factors responsible for the failure of the mechanical equation of state for creep. IN this report an attempt is made to correlate the creep properties of dilute a: solid solutions in aluminum with the subgrain structures that are developed during creep. The possibilities of such correlations have already been suggested by Wood et al. and others1-" who demonstrated that the subgrain structures are functions of the creep stress, creep strain, rate of creep, and temperature. Investigations by Sherby and Dorn' have shown that the creep strain, E, at constant load for dilute a solid solutions of aluminum is given by the functional relationship: e = f(8,u,) [1] where: 0 equals te-AH/RT = temperature-compensated time; t, time; AH, activation energy, - 35,800 cal per mol; R, gas constant; T, absolute temperature, above 400°K; and u,, initial creep stress. Consequently, it was anticipated that the subgrain structure that develops during a constant load creep test should also correlate with any two of the three significant variables C, 8, and Another possible correlation between the subgrain structure and the creep variables is obtained by differentiating Eq. 1 with respect to time, whence the creep rate, 2, becomes: = (2L) (2) =f (, u,) e-AHRT [2] or: e = F (c e H/RT, 0) [3] For the minimum creep rate, ;,, 8 is solely a function of U, as revealed by Eq. 1. Consequently, at the minimum creep rate Eq. 3 reduces to: = F (eAH/RT) [41 Correlations between U, and i, eAH/RT were found valid for solid solution alloys of aluminum where AH was a constant of about 35,800 cal per mol. The parameter ;, eH/RT is identical to the Zener-Hollo-mon parameter8," used by them in evaluating the tensile properties of copper and other metals. Eq. 4 suggests that the subgrain structure developed during secondary creep might be correlatable with either of the two variables 2, e H/RT or u,. Some of the solid solution aluminum alloys which were discussed in an earlier report' were also used in the present investigation. Sheets of these alloys were homogenized, cold rolled from 0.100 to 0.070 in. in thickness and then recrystallized to about the same grain size. Their chemical composition and grain size are recorded in Table I. Creep specimens were selected with their tensile axes in the rolling direction. The details for creep testing have been described10 and will not be repeated here. All creep tests were performed under constant load conditions. Experimental Results and Discussion Metallographic Structure of Creep Specimens: In order to obtain a preliminary concept of creep on the metallographic structure of high purity aluminum, the various ruptured specimens previously used to obtain the creep data for pure aluminum were polished and etched electrolytically in a dilute solution of fluoroboric acid. Oblique illumination was used to reveal the substructures which, for convenience, are shown in correlation with the vs. ;, eH/RT curve in Fig. 1. It is necessary to emphasize that the data for the curve refer to the various secondary stages of creep whereas the micrographs refer to the fractured creep specimens. Nevertheless a regular and systematic correlation is observed between E, eAH/RT (or the creep stress) and the micro-structure at fracture. For In (e, eAH/RT) = 42.3, which refers to creep at a high creep rate and a low creep temperature, the fractured aluminum specimen, as shown by the micrograph in the upper right-hand corner of Fig. 1, exhibited extensive deforma-

Jan 1, 1954

By J. Blodget Britton

To the question, "Do the Pennsylvania anthracites contain phosphorus ?" asked at the last meeting of the Institute during the discussion on the metallurgical value of Western lignites, I can now give a definite answer. Through the kindness of a gentleman connected with the Philadelphia and Reading Railroad, and another connected with one of the principal ironworks on the Lehigh, there was sent to the Iron-masters' Laboratory a number of samples of the coals now largely shipped from the Schuylkill and Lehigh regions. Seventeen of these I examined for their contents of ash and phosphorus, and obtained results as follows

Jan 1, 1873

By Charles Bohdanowicz

As in preceding years, the most intensive drilling activity during 1934 took place in the old fields of the western part of the Polish Carpathian petroleum province (district of Jaslo). The number of wells completed to the end of 1934, expressed in percentages, is as follows: Jaslo district, 57 per cent; oil fields outside Boryslaw-Tustanowice-Mraznica, 27; Stanislawow district 8 and Boryslaw fields only 7 per cent. The number of meters drilled (Table 2), expressed in percentages, for the same fields are as follows: Jaslo district, 51 per cent; oil fields outside Boryslaw-Tustanowice-Mraznica, 26; Stanislawow district, 12, and Boryslaw oil fields, 11 per cent. This comparison shows that most of the new

Jan 1, 1935

By Herbert Herman, M. E. Fine

THE first decomposition product of a supersaturated aluminum-rich A1-Ag alloy at low tempera- tures is Guinier-Preston zones.'-, The zones are ideal and each consists of a spherical shaped silver-rich cluster about 16 A in diam syrounded by a silver-poor shell approximately 72A in diam.' The composition of the two regions is not known with certainty., After quenching from the solution anneal, these zones form rapidly on aging at temperatures as low as -30°C.5 The rate of zone formation increases with aging temperature; the activation

Jan 1, 1961

By N. J. Grant, F. B. Cuff

DURING a recent investigation of high-purity aluminum,' evidence was found for grain-boundary sliding and migration at room temperature. The investigation was concerned primarily with an electron-microscopic study of a fine (approximately 1 micron) network that appeared on the surface of chemically polished aluminum. The nature of the network will not be discussed since it serves only as markers showing relative displacements in this instance. The pertinent observation, shown in Fig. 1, was made on a flat tensile specimen which had been strained about 8 pct at room temperature. As can be seen in this electron micrograph, a grain boundary has undergone a certain amount of sliding. The reason for the existence of the two differently appearing networks is given in the foregoing reference. For present purposes, however, the transition region can be disregarded. A close study of this picture reveals that in addi- tion to sliding there is a narrow band adjacent to and above the grain boundary. Fig. 2 is a schematic drawing showing the essential features of this band.

Jan 1, 1959

By J. W. Halley, G. L. Plimpton

Because of the two distinct stages in the solidification of rimmed steel, segregation in the rimmed ingot is more complex than that in the killed or semikilled ingot. In the earlier stage, chemical reactions, resulting in evolution of gas and vigorous stirring of the metal, effect a degree of negative segregation unique to rimmed steel. The composition of this zone constitutes the principal quality advantage of this type of steel. In the later stage of solidification, after the evolution of gas has ceased, the segregation follows the general pattern of a more completely deoxidized steel. However, the composition of the liquid remaining after the first solidification stage varies markedly from that of the original melt, some constituents having been partially removed as reaction products while the concentration of others has been intensified by rejection from the metal solidifying in the first zone. The aim, from the standpoint of segregation, in rimmed steel of high quality is to effect a maximum negative segregation in the rim zone without excessive concentration of undesirable elements at the center of the ingot. To achieve this aim, the composition of the melt may be varied and the furnace and pouring practice may be adjusted within certain limits. It is the purpose of this study to discuss segregation in rimmed steel from the standpoint of the mechanisms that produce it and to survey the phases of open-hearth practice that influence those mechanisms. Mechanisms Producing Segregation The mechanisms that determine the degree of segregation in the rimmed ingot are closely interrelated, making it difficult to select the primary factors and to determine a satisfactory order for presenting them. For instance, the question of sulphur segregation is relatively simple, since sulphur is not directly involved in chemical reactions in the ingot; but its concentration in the rim zone is dependent not only on its original analysis in the melt, its segregation coefficient, and the freezing rate, but also on the rate of its removal from the impure film on the solidifying surface. This washing action involves all the factors (such as freezing rate, the carbon-oxygen product, pressure, etc.) that determine the rate of gas evolution and hence the efficiency of film removal. Sulphur distribution between the rim and core is affected by the volumetric ratio between the two zones, and its segregation in the core is a function not only of the freezing rate of the core but also of all the foregoing factors that determine its concentration in the metal when solidification of the core starts. To simplify the presentation, it is proposed to treat the mechanisms affecting segregation independently in this section, reserving a discussion of their over-all effects for the section in which actual segregation data are given. The factors affecting segregation will be treated in the following order: (I) differential solidification, (2) removal of constituents as

Jan 1, 1945

By I. Lowthian Bell

THERE has been probably no improvement introduced into the manufacture of iron which created more surprise in the minds of practical smelters and of scientific men than Neilson's discovery of the hot blast. In 1829, Messrs. Dunlop & Co. consumed at the Clyde Works, near Glasgow, nearly 7 3/4 tons of coal to make a ton of pig iron, of which about 20 cwts. was employed under the boilers of the blowing engines, leaving nearly 7 tons for the consumption of the furnace itself. In the year 1833, by heating the air to 612° F. (322° C.), they reduced the 7 3/4 tons to 3 tons by the mere burning of 8 cwts. of coal in the apparatus for raising the blast to this temperature. The statement just given is strictly true in a commercial sense, but when we come to consider the question as one of physical science, it is necessary to eliminate some of the conditions which conduced to so extraordinary a result. Anterior to Neilson's time the fuel employed in smelting iron was coke, and it was supposed at that period, erroneously, however, that coal in its raw state, when burned with cold air, was totally unfit for the purpose in question. This mineral, as it was obtained from the Lanarkshire coal-field, contained about 35 per cent. of volatile matter, but the process of charring it was performed in so unskilful a manner that instead of receiving 88 cwts. of coke from 135 cwts. of coal, 60 cwts. only was the product of the operation. Again, the reduced consumption of carbon in the furnace itself was accompanied by a corresponding diminution of blast, and this was followed by an economy of half a ton in engine coal. After making a proper allowance, however, for all these collateral circumstances, we are within the mark when we admit that in actual coke, which is really the form the fuel has to assume before it is burnt in the blast-furnace, not less than 30 cwts. was saved by heating the blast to 615° F. (322° C.). This unexpected economy, be it remembered, was obtained by the combustion of the 8 cwts. of coal, somewhat wastefully applied in the hot-air apparatus. Numerous have been the opinions advanced by different authorities in the scientific world to account for the apparent anomaly, but none,

Jan 1, 1877

By A. K. Mukherjee, J. E. Dorn, J. D. Mole

Investigations were carried out on the effect of polyslip on the strain hardening of aluminum single crystals. The orientations investigated were those lor which the tensile axis was in the [001], [111], [112], and [012] directions plus another for which the Schmid angles for {111}(110) slip were 1 deg. The experimental data were analyzed on a model based on the intersection of dislocations with particular emphasis on the effect of polyslip on the activation volume for inter-section. It is shown that the rate of strain hardening inreases for those orientations wherein attractive dislocation intersections occur and that those orientations which produce the greater number of such intersections exhibit the greater strain hardening. Good correlation of the data is obtained with the concept that attractive junctions, as proposed by Saada, Play an important role in accounting for the rate of strain hardening. EXISTING concepts on the nature and cause of strain hardening in fcc metals have been deduced principally from experiments on the deformation of single crystals under single slip. The effect of crystal orientation on the shapes of the stress-strain curves for single slip have been summarized by seegerl and more recently by Clarebrough and Hargreaves.2 Tensile specimens whose axes fall near the center of the [001]-[011] line of the standard triangle of the stereographic projection exhibit the longest range of easy glide (Stage I) and the lowest rates of linear hardening (Stage 11) whereas specimens whose axes lie near fie [001]-[111] line of the standard triangle have limited or no easy-glide range and exhibit somewhat higher linear strain-hardening rates. Specimens whose axes lie near the [001] or the [ill] poles do not exhibit easy glide and have the highest rates of linear hardening. Kocks3 has shown that the highest rates of linear hardening Occur under Polyslip when the tensile axis coincides with the [111] or the [ 001] pole. Since the rate of strain hardening is sensitive to specimen orientation and the incidence of polyslip, these relationships might help to discriminate between various dislocation models for strain hardening in fcc metals. Previous attempts to analyze the effect of orientation on strain hardening,1"3 however, did not provide a unique answer to this problem. Consequently the present investigation was undertaken wherein additional data, particularly that for the effect of polyslip on the activation volume for intersection, was also determined in order to provide more complete information on the details of strain hardening. Whereas analyses of these data reveal that several recommended models for strain hardening are at variance with the facts, good correlation of the data is obtained with the concept that attractive junctions4 play an important role in accounting for the rate of strain hardening. I) EXPERIMENTAL APPROACH seegerl demonstrated that slip in fcc crystals at low temperatures is dependent on thermally activated intersection of glide dislocations with forest dislocations. This has been confirmed by tests on single crystals of aluminum by Mitra, Osborne and Dorn5 and on polycrystalline aluminum by Mitra and Darn.' Thus in accord with Seeger's theory, the shear strain rate, ?, below a critical temperature, T, is where .V is the number of points of contact per unit volume between forest dislocations and glide dislocations, A is the area swept out per successful intersection, b is the Burgers vector, v is the frequency of vibration of the segment of the glide dislocation undertaking intersection, U is the activation energy for intersection, k is Boltzmann's constant, and T is the absolute temperature. For aluminum, which has an extremely high staeking-fault energy, the constriction energy is negligibly small and therefore the activation energy decreases practically linearly with the stress according to as will be recomfirmed later, where Uo is jog energy at the absolute zero, G and Go are the shear moduli at the test temperature T and O°K, respectively, L is the spacing of the forest dislocations, t is the applied shear stress for slip, and tGo is the stress field that must be surmounted athermally.

Jan 1, 1965

By J. Brett, S. Friedman

A study of the diffusion of nickel into both fibrous and recrystallized 0.065-in.-diam silica-alumina doped tungsten wire at 1200°C has been conducted. The diffusion profiles were determined by chemical dissolulion of successive circumferential layers and spectro-photometric determination of nickel in the etchant. It was shown that the diffusion of nickel into tungsten is markedly structure-sensitive. No significant amount of nickel could be introduced at 1200°C into tungsten which had first been recrystallized at temperatures of 2300°C, leading to an upper limit estimate for the bulk diffusivity of nickel in tungsten of 10-11 sq cm per sec at 1200°C. However, nickel did diffuse into initially fibrous wires, caused re crystallization, and was alsays present at the advancing recrystallization front. The accumulation of nickel in an initially fibrous region ceases when the recrystallization front arrives. The characteristics of the resulting diffusion profiles are explained in terms of the relation between diffusion processes and micro structural changes. WHILE it is well-known that the presence of nickel and certain other metals causes low-temperature recrystallization of the cold-worked fibrous structure of doped tungsten,''' the character of the phenomenon is not well understood. Recently it was shown that the recrystallization reaction can be induced at low temperatures by the presence of solid nickel on the surface of doped wire, but not by exposure to nickel vapors.3 Once recrystallization was initiated, a continued source of nickel was required for propagation of the recrystallization front. The phenomenon appeared to be a complicated solid-state reaction since, in addition to the change in structure of the tungsten from fibrous to equiaxed grains, diffusion of nickel from the surface into the recrystallized and fibrous structures was occurring with possible chemical reaction between nickel and tungsten at the surface and interaction of nickel with the dopants which ordinarily stabilize the fibrous structure within the wire. The objective of the present work was to study the diffusion of nickel into fibrous and recrystallized tungsten structures in order to clarify the relationship of the diffusion process to nickel-induced recrystallization. Studies of interdiffusion in the Ni-W system4"7 have been principally concerned with the mobility of tungsten in nickel. Information on diffusion of nickel in tungsten is meager, and there seem to be no studies of the mobility of nickel in tungsten which elucidate the structural aspects of the phenomenon. The present experiments were designed to determine the diffusivity of nickel at 1200°C in fibrous tungsten, in large-grained tungsten prerecrystallized at high tem- perature, and in tungsten recrystallized at 1200°C due to the presence of nickel. Although the concentration profiles were determined in these experiments, unexpected changes in boundary conditions or complex diffusion paths complicated the analysis of these profiles so that the interpretation could not be readily expressed in terms of simple diffusivities. EXPERIMENTAL PROCEDURE The experiments were conducted on Sylvania 0.065-in.-diam silica-alumina doped commercial tungsten wire, hereafter designated as ordinary doped wire. A special lot of 0.065-in.-diam silica-alumina doped low-nickel wire was also used. Impurity analyses of the wire are given in Table I. The experimental design is shown in Fig. 1. All heat treatments were conducted in vacuum. Two groups of ordinary doped wire were prepared for diffusion with nickel. One group in the as-received (fibrous) condition was elec-tropolished, nickel-plated, and annealed at 1200°C for 20 and 40 hr, or was exposed to nickel vapor at 1200°C for 20 and 40 hr. The second group was recrystallized to an equiaxed grain structure at 2300°C for 3 hr, electropolished, nickel-plated, or exposed to nickel vapor for anneals at 1200°C for 20 and 40 hr.

Jan 1, 1969

By R. L. Curfman

WHEN the Uranium Reduction Co. mill was put on stream in October 1956, one of the many operational problems was that the sand-slime separation circuits could not produce a satisfactory RIP feed, inasmuch as production greatly exceeded de- sign capacity. The original cyclone portion of the circuits consisted of two stages of three 14-in. cyclones in each circuit, as shown in the condensed flowsheet. The high percentage of +325 mesh material in the over- flows of these 14-in. cyclones was not consistent with good operation, and flow rates per ton of ore were high, indicating that not enough of the total solids in the ore was being rejected as sands. It was inferred by members of the metallurgical department that returning the underflows, or sand fraction, from these cyclones back into the drag classifiers was the primary reason for dirty feed.

Jan 7, 1958

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By Strathmore R. B. Cooke, Paul B. Queneau

The kinetics of the dissolution of scheelite in basic solutions of carbonate and fluoride were investigated. Work was also done with solutions of alkali metal chloride, hydroxide, phosphate, and mixtures of phosphate and fluoride. The study was conducted at 90 psig and at temperatures ranging from 100" to 155"C, and both natural and synthetic scheelite single crystals were used. The interaction of scheelite with carbonate solutions generally followed a parabolic rate law, and resulted in the formation of calcite crystals on the attached surface. The transport of the CO3 through the calcite to the scheelite surface was probably rate -controlling between 115" and 135°C. Positive deviations from Parabolic behavior were observed at 100" and 155?C, presumably due to the calcite grain growth, and to the formation of a noncoherent calcite layer, respectively. The leaching of scheelite with alkaline fluoride solution produced a calcium fluoride reaction-product which covered the surface as a sheet-like layer. Below 110°C the dissolution rate was parabolic; at 115" and 135°C it was linear. In the linear region, the periphery of the calcium fluoride layer lifted from the sample. Only the lower layers, braced by the scheelite substratum, remained unbroken. This bound layer, approximately constant in thickness, limited the rate at which the fluoride could attack the scheelite. The phosphate and phosphate-fluoride leaches dissolved scheelite at a linear rate; solid reaction products were respectively hydroxyapatite and fluorapatite. Sodium hydroxide and chloride were not effective leachants, and did not produce observable solid reaction products. THE feasibility of pressure leaching of scheelite pulps with basic solutions containing either carbonate or fluoride ions, as indicated by the following equations, has been established by previous investigators:1-3 200°C CaWO4s + CO37q - CaCO3s+WO4aq [1] 200°C CaWO4s + 2Faq ^ CaF2s+WO4aq [2] It is to be noted that a commercial process employing reaction [I] is in use at Union Carbide's operation near Bishop, Calif. In the earlier work referred to, it was apparent that the precipitation of the solid reaction-product on the scheelite particles sharply reduced contact of the leachant with the scheelite. We have extended this work by studying the kinetics of dissolution employing single crystals of scheelite of known exposed surface area. In addition, the effectiveness of solutions of phosphate, of phosphate with fluoride, and of chloride and hydroxide as leachants for scheelite have been investigated. EXPERIMENTAL Apparatus. The low-pressure autoclave used in this wo (100 psig maximum) is essentially that of J. Halpern4 as modified by F. A. Forward.5 Constructed entirely of 316 stainless steel, its maximum capacity is 4000 ml. The temperature in the autoclave was regulated to *0.5?C by a Wheelco thermocouple controller. A 4-in. diam, three-bladed impeller, circulated solution upward against the sample, and a strobo-scope permitted holding the stirring rate to *15 rpm. A check valve and a "pop" type safety valve were installed, a sample holder was fixed to an externally adjustable rod, and a water-cooled condenser was placed in series with the sampling valve. The stainless steel sample holder, Fig. 1, held the epoxy-mounted sample (f) five mm above the impeller. Tightening the tapered sleeve (d) positioned the epoxy-resin specimen-mount by forcing it back against the spacer (c). The mount (e) was 1 in. diam. Sample Description and Preparation. Both synthetic and natural scheelite crystals were leached. The former were single crystals of 99.95 pct purity which were leached approximately perpendicular to the "c" axis; they were supplied by the Gallard-Schlesinger Chemical Manufacturing Corp. The natural crystals, supplied by Minerals Unlimited, were transparent, analyzed 99.8 pct CaWO4, and in ultraviolet illumination exhibited the characteristic blue glow of substantially molybdenum-free scheelite. To permit exposure of an essentially constant surface area of scheelite to the leachant, the samples were mounted in Scotchcast Brand Resin No. 250 (Minnesota Mining and Manufacturing Co.). The mount-

Jan 1, 1970

By H. R. Deeth, C. J. Koenig

About ten years ago nepheline syenite was introduced to the ceramic industry and the material has now found application in the various branches of the industry, namely, as a vitrifying agent in white-wares and as a source of alumina and alkalies in glasses, glazes, and porcelain enamels. Spencel described the early mining and processing developments regarding this material. Since the time of his article many research papers have appeared relating to the usage of nepheline syenite but little has been published relative to subsequent mining and processing methods. A complete indexed review of the literature was issued recently by Ohio State University.2 Since "Lakefield" nepheline syenite from Blue Mountain, Ontario (Fig I); is the only commercial ceramic-grade nepheline syenite now being marketed on this continent, discussion is limited to this operation carried on by American Nepheline Limited, Lakefield, Ont., and its subsidiary in the United States, American Nepheline Cory. at Rochester, N. Y. The Deposit Blue Mountain is a long ridge rising to an elevation of about 350 ft at its highest point above the surrounding country and extending for about six miles in a northeasterly direction across Methuen township, Peterborough County. The rock of the Blue Mountain central alkaline intrusive is fine grained, light colored and of even granitic texture. The solidified mass consists predominately of the minerals albite, nepheline and microcline in order of abundance. The average mineralogical composition for the deposit obtained by a study of 112 samples taken regularly over the whole formation is as follows:3 Volumetric Mineral Per Cent Albite.................... 54 Microcline................ 20 Nepheline................ 22 Muscovite................ 2 Mafics.................... 2 (Biotite, hastingsite, magnetite) Total................... loo The mineral nepheline (or nephelite) belongs to the feldspathoid group but is lower in silica content than are the feldspars. It is a silicate of soda, potash, and alumina (NaKAl2O32SiO2). Its presence with albite (Na2oA12O3 6SiO2) and microcline (K2O A12O3 6SiO2) gives the Blue Mountain deposit an alkali content of 15 pct and an alumina content of approximately 24 pct. While this huge alkaline mass is somewhat variable mineralogically, it has a uniform chemical composition. When the iron, mostly in the form of magnetite, is removed during processing, a remarkably uniform finished product is obtained. Geological surveying has disclosed many million tons of nepheline syenite in the Blue Mountain deposit. Diamond drilling in the area where mining is now being carried out indicates a block of about one million tons.

Jan 1, 1949

By S. S. Cole, H. Sigurdson

The melting points of mixtures of titanium dioxide and other titanates have been reported to a limited extent as binary systems and some results have been reported in conjunction with silicon dioxide. The limited data indicated that a low melting zone might exist in a ternary or quarternary system of CaO-MgO-TiO2-Al2O3, since the eutectics reported in the binary systems of MgO.TiO2-TiO2, Al2O3TiO2-TiO2 and CaO.TiO2-TiO2 were of about equivalent composition of TiO2. The importance of a low melting region with a high titanium oxide value in the developing of high titanium slags is fully appreciated by metallurgists. A comprehensive study was undertaken to establish basic information on low melting titanate mixtures. Compounds in the System CaO-MgO-TiO2 -Al2O3 Preparation of the titanates of CaO, MgO and Al2O3 confirmed reported data that the following compounds could be formed under oxidizing conditions in solid state reactions: CaO.TiO2, 2MgO.TiO2, MgO.TiO2, MgO-2TiO2 and Al2O3.TiO2. Under oxidizing conditions it was not possible to react MgO with TiO2 in mol ratios higher than 1:2 without having unreacted TiO2 in the product, nor was it possible to form calcium or aluminum titanates with a higher mol ratio of CaO and A12O3 to TiO2 than 1:1. By fusing mixtures of Al2O3-TiO2 and MgO-2TiO2 together a series of solid solution products were obtained, which showed an MgO-2TiO2 X ray diffraction pattern shifted to smaller inter-planar spacings. Range of Investigation Data in the literature1 indicated that these titanates had melting points which ranged from 1645 to 1860°C. Since the purpose of the study was primarily to provide useful data for smelting titaniferous ores, the work was restricted to the zone of the system which would include the crystalline phases present in the slags. The explored limits were bounded by CaO.-TiO2-MgO.TiO2-TiO2in the base plane. The system was extended to a fourth component Al2O3-TiO2 since many titaniferous ores contain appreciable amounts of A12O3. In the quarternary system CaO-TiO2-MgOTiO2-TiO2-Al2O3TiO2, a tetrahedron was used to represent graphically the components, with one component at each point of the tetrahedron. In the base plane, mixtures were pre- pared to represent fairly uniform changes of composition over the desired range expressed on a mol percent basis. Al2O3-TiO2 was brought into the system in increments of 10 mol pct up to 40 pct. Mixtures were then made up for each of the Al2O3-TiO2 planes. The ranges employed were then represented by five planes cutting the tetrahedron at 10 mol pct Al2O3-TiO2 intervals. Choice of Equipment Although it was necessary for all smelting work to be done in a strongly reducing atmosphere, it was decided that all melting point determinations should be done under oxidizing conditions. This decision was prompted by the fact that TiO2 reduced to lower oxides in a reducing atmosphere with consequent changes in melting points. The use of a micropyrometer and a platinum strip furnace for work of this type is adequately described in the literature.2 With modifications, equipment was selected which provided a fairly rapid method of determining melting points of refractory oxides. The final assembly, which was used, consisted of a platinum strip furnace and a Leeds and Northrup disappearing filament optical pyrometer attached to a special telescope which magnified the sample about 20 diam. The furnace assembly consisted of a platinum strip 0.005 X 0.3 X 2.2 in. mounted on brass posts on a refractory base. This was enclosed in a black steel shell which had a 2-in. opening at the top for purposes of sighting the telescope. The platinum strip was in series with two 0.04 ohm nichrome resistors connected to the secondary of a 2 kw transformer which supplied 17 volts. The current to the primary was varied

Jan 1, 1950

By Walter R. Hibbard

THE term lineage was first introduced by Buerger1 to denote dendritic branches, grown from a crystal nucleus during solidification from the liquid, with imperfections in alignment of the order of 10-1 [ ] to 10-4 cm. These imperfections are associated with distortions of the dendrites caused by the subsequent solidification of the inter-dendritic filling and are illustrated in Fig 11. Buerger etched zinc single crystals made by the Bridgman2 method to develop this dendritic pattern and show lineage microscopically. Since maximum crystal growth in face-centered cubic metals occurs along the [100] directions,2 lineage would appear in copper as small deviations of dendritic branches from these directions. Elam4 and others5-8 reported etching effects resulting from coring along the cube face traces of various copper alloy crystals. These traces were used by Samans8 to orient single crystals. Williamson9 noted a "lined structure (in alpha brass single crystals) consisting of an ordered arrangement of etch pits" which were probably traces of {100} planes but somewhat uncertain because they were never straight (i.e., apparently lineage). Greninger10 described the distortion and multiplicity of Laue spots in back reflection X ray photograms of copper single crystals showing lineage. The present investigation includes metallographic, X ray and property studies of lineage in large grain and single crystal specimens of copper. PREPARATION OF SPECIMENS Specimens 10 in. long and ½ in. diam of oxygen-free copper (O.F.H.C.) (99.985 pct) were melted vertically in graphite crucibles under an atmosphere of commercial nitrogen purified through a gas train including sulfuric acid, potassium chloride, magnesium chlorate, hot copper chips and phosphorus pentoxide. After a temperature of 1200°C had been maintained for ½ hr, the furnace was turned off and the specimens cooled at a rate of about 150°C an hour. This method of direct solidification was used by Greninger10 to produce single crystals with marked lineage and in this investigation produced a fair yield of single crystal specimens in

Jan 1, 1947

By B. Foley

IN THE first report1 disks of steel of known composition and history were exposed, under carefully prescribed conditions, to impacts of explosion products resulting from the explosion of 50-gm. charges of explosives having well-determined rates of detonation, or to impacts of a weight of known mass, falling through measured distances. There were available at the Bureau of Mines Experiment Station five explosives, having rates of detonation of 5716, 4470, 3190, 2296, and 1523 meters per second. It being desired to continue this exposure downward, and no explosives with a lesser rate of detonation being at hand, resort was had to the impact of a falling weight, the differences in the velocity of impact being attained by varying the height from which the weight was allowed to fall. It was expected by this means to demonstrate experimentally that the development of Neumann bands was determined by the suddenness of the deformation of the metal in which they were produced. But while progressive deformations were obtained with the explosive arges, the falling-weight method failed because the tup was ogressively deformed, also the disks were so flattened as to be unfit for metallographic examination. A return, therefore, has been made to the use of explosives as the source of energy, an air-gap being interposed between the charge of explosive and the disk, as the effect diminishes as the function of the distance between the charge and the object on which the products of its explosion, or the shock wave from its detonation, impinge. The details of the arrangement of the tests by the air-gap method were the same as those described by Foley and Howell,2 except that after the system had been set up and the desired apparent specific gravity for the explosive

Jan 2, 1926

By Joseph Fry, Ralph H. Espach

In the spring of 1943, when it was evident that the Tensleep bandstone in the Elk Basin Field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes. of gas in solution. saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep Reservoir of the Elk Basin Field has unusually varying physiral characteristics, such as a saturation pressure of 1,250 psia and 490 cu ft of gas in solultion in a barrel of oil at the crest of the structure and a saturation pressure of 530 psia and 134 cu ft of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the gas in solution in the oil varies from 18 per cent for oil on the crest to 5 per cent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of the oil in the structure. Many geologists and petroleum engineers have considered that all the oil in a petroleum reservoir has rather uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas; that such is not always so is borne out by the results of the study by the writers. INTRODUCTION The Rocky Mountain region is one in which may be found striking examples of the unusual in oil and gas accumulations, as is evident from the following: The high helium content (7.6 per cent) of the gas in the Ouray-Leadville limestone sequence in the Rattlesnake Field, New Mexico, and gases of similar helium content in other fields; 50" to 55' API gravity distillate in solution in carbon dioxide gas and recoverable through retrograde condensation, in the North McCallum Field, Colorado; the occurrence of gas, oil, or both in closely related structures contrary to the usual concepts of gravimetric segregation: the accumulation of gas and/or oil in structures closely related to other structures that apparently are more favorable but do not contain oil or gas accumulations; the high hydrogen sulfide content (as high as 42 per cent) of the gas associated with oil in some fields in the Big Horn Basin, Wyoming; and the wide range of fluid chararteristics found in the Elk Basin reservoir. Elk Basin, an interesting old oil field that has been producing oil from the Frontier formation since 1915, is situated in a highly eroded basin resulting from the erosion of the crest of an anticline and some of the underlying softer shales. The field came back into national prominence during 1943 when it became known that it was the largest single reserve of new oil discovered in the United States that year. The Tensleep sandstone was found to contain oil in November. 1942, when a well drilled to a depth of 4,538 ft (44 ft into the Tensleep sandstone) flowed oil at the rate of 2,500 B/D. By the end of 1949, 137 oil-producing wells and five dry holes had been drilled, and approximately 32 million bbl of oil had been produced. Approximately 6,000 acres may be considered productive of oil in the Tensleep Reservoir, and estimates of the oil that will be produced average 200 million bbl. The Tensleep Reservoir has further interest because it ha-greater closure than any oil field in the Rocky Mountain region; the closure of the Elk Basin anticline is variously estimated at 5.000 to 10,000 ft. of which the top 2.00 ft of the structure contained oil. SUBSURFACE OIL SAMPLING Fig. 1 is a structural map of the Elk Basin Tensleep Reservoir, on which the nine wells used in this study and the numbers correvponding to the well designations hereafter referred to are shown. Wells 1. 2, 3, 4, and 8 were tested and sampled during October and November. 1943. and Wells 5, 6. 7, and 9 during June and July, 1944. An electromagnetic type sampler developed by the Bureau of Mines and described by Grandone and Cook' was used in obtaining the subsurface oil samples. As the wells were tubed nearly to bottom, the sampler was run as far as possible in the tubing hut never below the top perforations. The following procedure was used in testing and sampling the wells: A well was shut in for at least three days, after

Jan 1, 1951