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By Charles White Merrill, James W. Pennington

No metallurgical process developed in the 20th century compares with froth flotation in its effect on the mineral industry. Processes like gravity - concentration, amalgamation, and pyrometallurgical reduction are of ancient origin; others like cyanidation and electrolytic reduction were well established by 1900. Such metallurgical processes as heavy-media separation, ion-exchange, and solvent extraction belong to this century, but their influence is small compared with froth flotation. Data collected by the U. S. Bureau of Mines* in a canvass of 202 froth flotation plants reveal that, in 1960, 198- million tons of material was treated to recover 20-million tons of concentrates which contained approximately $1 billion in recoverable products. SIGNIFICANCE OF FLOTATION Froth flotation as described in this chapter refers to a wet process for separating properly ground mineral particles into two or more products. It involves the separation of mineral particles from each other in a liquid pulp by means of air bubbles. Finely crushed ore is agitated in water with the addition of air or other gases. Various chemicals and oils are added to cause the selected mineral particles to attach themselves to the air or gas bubbles. These bubbles, carrying the mineral particles, rise to the surface where they are removed in a froth, while the other particles remain suspended in the pulp. The earliest flotation divided the raw material into two products: a bulk concentrate that was removed as a froth and a tailing that remained in the flotation machine. The froth usually contained the valuable constituents. The successful application of such a process depended on the recovery of a single concentrate from which one or more valuable constituents could be recovered by a chemical or smelting process. With the advance of the art, however, the principle of selective flotation, by which two or more relatively pure products could be recovered from complex raw materials, was evolved. Other chapters in this volume describe the developments during the last 50

Jan 1, 1962

By R. P. E. Hermsdorf

THE electrolytic refining of metals for the removal of undesirable impurities has become a recognized necessity in the nonferrous field. Copper, lead, zinc, nickel, silver and gold have been produced in this manner for years. The United States Metals Refining Co., realizing that considerable quantities of lead and tin could be made available to the trade if a satisfactory method of purification of these metals could be established, decided to investigate the possibilities of electrolytic solder. In cooperation with Dr. Edward F. Kern, of the School of Mines at Columbia University, the company developed a process of electrolytic refining of lead-tin alloys using a tin-lead fluosilicate electrolyte. A pilot plant was installed in November, 1927, and the commercial unit was put in October, 1929. Since that time thousands of tons of electrolytic solder have been produced in this plant and consumed by all branches of industry that use solder.

Jan 1, 1936

By J. H. Nelson

An outline survey of the economic outlook for the United States export trade in petroleum products resolves itself broadly into two general divisions; first, a consideration of our present position in this trade, and second, a discussion of the visible factors which promise to affect appreciable changes in the immediate future in that trade. The United States PetRoleum Exports of majoR Petroleum Products 1925, 1926 and 1927

Jan 1, 1928

By R. F. Mehl, B. Lustman

The formation of intermediate phase layers in cementation processes has been subjected to extensive qualitative investigation though to relatively little quantitative study; this work has recently been fully summarized by F. N. Rhines.' It is necessary here only to cnumerate the general conclusions drawn concerning the kinetic laws governing the growth of intermediate layers and to state what is known concerning the structural changes accompanying the generation of phase layers. I. When the intermediate phase is protective in type—i.e., when its density is less than that of the base metal, so that a continuous coating is formed and maintained—the isothermal growth of the phase follows a simple parabolic equation: X2 = kt [i] where X is the thickness of the alloy layer, k thc reaction rate constant, and t the time. The applicability of this equation to diffusion processes is tested by plotting the square of the thickness versus time, or by plotting the thickness versus the square root of time; the resultant achievement of a straight line in such a plot has been considered sufficient proof of the validity of this equation. Exceptions have been found where liquid phases are involved in the reaction, where the diffusion layer is cracked,2 and where thin semimetallic oxide and sulphide coatings are formed on metals.$ In the first two cases the thickness increases linearly with time, and in the latter it is a logarithmic function of time. 2. The rate of thickening varics with temperature according to the Arrhenius equation: k = Ae-Q/RT [2] where k is the parabolic rate constant of Eq. I, or some other rate-descriptive function, A is the action constant, e the base of natural logarithms, Q the heat of activation, R the gas constant, and T absolute temperature. This equation has been found to be generally valid except when transformations occur during reaction in either the base metal or in the reaction layer; in such instances Eq. 2 is still applicable with different values for the constants A and Q above and below the transformation temperature. 3. Ali phases that are stable at the temperature at which diffusion occurs will appear in the interdiffusion of two components. In some cases certain of the phases may be too thin to be observed and identified easily. Nonequilibrium phases have never been noted in thick reaction layers; i.e., layers of a thickness that may be discerned microscopically. The relative thickness of each phase in a diffusion layer is proportional to the concentration gradient and to the rate of diffusion in that phase.4 The reaction layers tend to have a

Jan 1, 1942

By Lawrence Adler

In-situ rock has well-recognized rupture and yielding responses. Attention is called to an intermediate response, granulation, which consists of an evenly distributed, small-scale crumbling accompanied by swelling. Granulation results in a negative slope for the inelastic portion of the stress-strain curve as successive interlocks are destroyed, and the load-carrying capacity of the material is reduced. Volumetric swelling with softening also takes place. The prerequisites for such a response are moderate confinement and a uniformly distributed defect pattern. Since rock masses, as well as rock as an intact material, have such patterns in their jointing and texture, respectively, granulation is characteristic of them. The presence of granulation can be demonstrated for a very wide scale, ranging from laboratory testing to regional geologic phenomena. The response of an engineered structure is considered in detail. Granulation appears to be dependent upon internal moments, the formation of which can be controlled by engineering design. The practical implications of such control can be significant in optimizing underground instability and in improving excavation techniques. Rock is usually considered to behave inelastically under high load, by fracturing as a brittle material, or by yielding as a ductile material, ignoring time dependency. These responses, which are characteristic of metallic behavior, appear idealized in Fig. 1, where linear-elasticity approximates the initial behavior. However, another major deformation mechanism peculiar to rock has long been recognized in geology, the granulation of an interlocked material. Granulation consists of a uniformly distributed fracturing and crumbling of the material, accompanied by swelling and softening. Predictably, the associated inelastic portion of the load-deformation curve has a negative slope,

Jan 1, 1971

By Jo. E. Sheridan

The Dawson coal-mines are owned aid operated by the Stag Canon Fuel Co., of which Dr. James Douglas is President and E. L. Carpenter general manager. The property is situated in Colfax county, N. M., and the openings now in operation are in townships 28 and 29 N R. 20 E., and township 28 N E. 21 E., shown in Fig. I. The mines are part of the southern end of the Raton coal-field, which extends north into Colorado and embraces many coal-camps of the Trinidad section. II. Geology. Geologically, the coal-measures, commonly known as the Laramie series of the Cretaceous system, have x thickness of about 800 ft. in the vicinity of Damson. The coal makes an excellent coke, and, according to some authorities, its coking properties are due to the action of intruded sheets and sills of igneous rock, the sheets occasionally thickening into masses resembling laccoliths, at such places making nearer approach to the coal and sometimes producing small areas of natural coke. There are but few dikes throughout the entire southern portion of the field and little or no faulting along the dikes. In some parts of this great coal-field the intrusive sheets are far removed in the green shales below the coal-measures, and are so much altered as to be difficult of identification. There is but little disturbance of the strata throughout the Raton coal-field in as far as it extends into New Mexico. There are two workable seams in the coal-measures, and two or three smaller coal-seams, ranging from 1 to 2.5 ft. in thick-

Jan 1, 1910

By E. A. Gulbransen, J. W. Hickman

ONE of the important factors that determine the resistance of a metal or alloy to further chemical reaction is the structure of the superficial oxide film A thorough understanding of the physical and chemical structure as well as the stability of the oxide film formed on the surface as a function of time and temperature of the chemical reaction might furnish clues as to the nature of the reaction process and the protective nature of the film A comprehensive program has been undertaken to study these phenomena This paper summarizes the structure of the oxide films formed on the metals iron, cobalt, nickel, chromium and copper at temperatures up to 700°C Before the introduction of the electron diffraction technique, it «as necessary to use either direct chemical analyses or X-ray diffraction analyses to determine the nature of the oxide film formed on the metal or alloy Chemical analyses yields information on the percentages of the several atomic species present in the film while X-ray diffraction analyses yield information on the atomic geometry In special cases the information obtained may be identical, but in general both view-points are necessary Much of, the early work was carried out on the oxidation of bulk samples where thick films were obtained The products were identified after cooling to room temperature by X-ray diffraction and chemical analyses Although much useful information has been obtained in this manner, little could be learned about the character of the protective oxides during the period when the films were actually protective Evidence concerning the chemical structure of thin oxide films has been made possible by the development of the electron diffraction reflection technique In this method the most fruitful investigations have been made by carrying out the reaction in situ at the temperature at which the film is actually protective LITERATURE The oxidation of iron has been extensively investigated by X-ray and electron diffraction Jackson and Quarrell1 found that oxide films formed and examined at the same temperature differed considerably from those allowed to cool to room temperature The results showed that below 400°C the oxide that was stable in intimate contact with iron was Fe304, between 515° and 900°C the stable film was FeO Above the upper change point of iron the oxide was found to be Fe304 prom 400° to 515°C , FeO, Fe304 or a mixture of the two oxides was found Recrystallization of the air-formed film below 400° and above 900°C led to the formation of Fe304 In the range where thicker films consisted of FeO, the air-formed film was converted to a new hexagonal oxide not previously described

Jan 1, 1946

By R. F. Mehl, B. Lustman

The formation of intermediate phase layers in cementation processes has been subjected to extensive qualitative investigation though to relatively little quantitative study; this work has recently been fully summarized by F. N. Rhines.' It is necessary here only to cnumerate the general conclusions drawn concerning the kinetic laws governing the growth of intermediate layers and to state what is known concerning the structural changes accompanying the generation of phase layers. I. When the intermediate phase is protective in type—i.e., when its density is less than that of the base metal, so that a continuous coating is formed and maintained—the isothermal growth of the phase follows a simple parabolic equation: X2 = kt [i] where X is the thickness of the alloy layer, k thc reaction rate constant, and t the time. The applicability of this equation to diffusion processes is tested by plotting the square of the thickness versus time, or by plotting the thickness versus the square root of time; the resultant achievement of a straight line in such a plot has been considered sufficient proof of the validity of this equation. Exceptions have been found where liquid phases are involved in the reaction, where the diffusion layer is cracked,2 and where thin semimetallic oxide and sulphide coatings are formed on metals.$ In the first two cases the thickness increases linearly with time, and in the latter it is a logarithmic function of time. 2. The rate of thickening varics with temperature according to the Arrhenius equation: k = Ae-Q/RT [2] where k is the parabolic rate constant of Eq. I, or some other rate-descriptive function, A is the action constant, e the base of natural logarithms, Q the heat of activation, R the gas constant, and T absolute temperature. This equation has been found to be generally valid except when transformations occur during reaction in either the base metal or in the reaction layer; in such instances Eq. 2 is still applicable with different values for the constants A and Q above and below the transformation temperature. 3. Ali phases that are stable at the temperature at which diffusion occurs will appear in the interdiffusion of two components. In some cases certain of the phases may be too thin to be observed and identified easily. Nonequilibrium phases have never been noted in thick reaction layers; i.e., layers of a thickness that may be discerned microscopically. The relative thickness of each phase in a diffusion layer is proportional to the concentration gradient and to the rate of diffusion in that phase.4 The reaction layers tend to have a

Jan 1, 1942

By A. W. Peake, F. O. Prior

Considering the great advance in the development and application of electricity, it is not strange that eventually a big field for its use has been found in oil-field operations. So far as is known, the first electric drive in oil-field operations was in the Russian field of Baku in 1900. The first application in this country was made by the South Penn Oil Co. near Folsom, West Va. in 1903. In 1916, electric power was first used in the Burma fields of India for drilling and pumping. Between 1916 and 1922, The Empire Gas & Fuel Co. made the first large electrical installation in the Mid-Continent fields. But although the first application was made 27 years ago, it is only within the last 10 years that oil companies have begun to look upon its use with much favor. Within the last few years, there has been a steady increase in the use of electricity in the oil fields. The first application of electricity for oil-field operations in Wyoming was in the Lander field in 1919; the second was in 1924 in Salt Creek; and the third, and last to date, was made by the Continental Oil Co. in the Big Muddy field during 1926. Lander Field The electrification of oil-field operations in Wyoming was initiated by J. W. Steele, superintendent of the Producers & Refiners Oil Corpn., in the Lander field in 1919. At that time, 32 wells were being pumped from five band-wheel powers, with oil engines as the prime movers. Eight barrels of fuel oil were used for power per day and at the price of 90 c. per bbl. the fuel bill was $36 per day. It was decided to try a 15 to 35-hp. oil-field motor on one of these powers. Electric power was generated with steam at the old Wind River refinery station. This test was so successful that in 1920 all five powers were equipped with 15 to 35-hp. oil-field motors, the power being obtained from the Sinks Canyon hydroelectric station. Four of these powers pumped wells at an average depth of 1450 ft., and the fifth pumped wells at an average of 2100 ft. In 1920, the average production per day from the 32 wells was 325 bbl. The power bill on the

Jan 1, 1928

By M. W. Ditto

THe conversion of the beehive coke plants, in this country, to byproduct plants has been slow, because the coal supplies were near the centers of the steel industry. With the growth of this industry, especially with its development around Chicago, it became necessary to transport large tonnages of coal from the eastern districts and then convert it into coke. The losses due to transportation costs were partly offset by the value of the byproducts recovered. To save the transportation costs, it was desirable that the coal deposits of Indiana and Illinois be utilized. This coal had always been classified as non-coking; it was also considered unsuitable for the metallurgical field because of the high ash and sulfur contents. The conditions, however, were promising enough to start experimental and development work, which crystallized in the design of the Roberts coke oven. The fundamental features of most coke ovens, with respect to the application of heating gas and the recovery of byproducts, are the same and, in the last few years, the tendency has been toward the better application of heating to the walls, higher thermal efficiency, and, by the control of heating conditions, the increase of byproduct yields. Structural features also have been improved and the use of high-grade refractory material has allowed the use of higher temperatures with the resulting higher rated capacity per oven per day. Great improvements have been made in both recuperators and regenerators, particularly with reference to the individualizing of each oven with respect to its adjacent oven, so that each can be operated as a unit if desired. The highest development of the flue type of oven has been applying individual regenerators for the recovery of waste heat. After some research work, it was found that the high-volatile Illinois coals could be utilized for coke by obtaining the better application and control of the heating conditions in the oven. Most of this high-volatile coal that had been used gave a good coke structure under certain conditions. The fact that coke was occasionally made from this coal, demonstrated the possibiity of making coke from it at all times pro-

Jan 1, 1923

By M. W. Ditto

THe conversion of the beehive coke plants, in this country, to byproduct plants has been slow, because the coal supplies were near the centers of the steel industry. With the growth of this industry, especially with its development around Chicago, it became necessary to transport large tonnages of coal from the eastern districts and then convert it into coke. The losses due to transportation costs were partly offset by the value of the byproducts recovered. To save the transportation costs, it was desirable that the coal deposits of Indiana and Illinois be utilized. This coal had always been classified as non-coking; it was also considered unsuitable for the metallurgical field because of the high ash and sulfur contents. The conditions, however, were promising enough to start experimental and development work, which crystallized in the design of the Roberts coke oven. The fundamental features of most coke ovens, with respect to the application of heating gas and the recovery of byproducts, are the same and, in the last few years, the tendency has been toward the better application of heating to the walls, higher thermal efficiency, and, by the control of heating conditions, the increase of byproduct yields. Structural features also have been improved and the use of high-grade refractory material has allowed the use of higher temperatures with the resulting higher rated capacity per oven per day. Great improvements have been made in both recuperators and regenerators, particularly with reference to the individualizing of each oven with respect to its adjacent oven, so that each can be operated as a unit if desired. The highest development of the flue type of oven has been applying individual regenerators for the recovery of waste heat. After some research work, it was found that the high-volatile Illinois coals could be utilized for coke by obtaining the better application and control of the heating conditions in the oven. Most of this high-volatile coal that had been used gave a good coke structure under certain conditions. The fact that coke was occasionally made from this coal, demonstrated the possibiity of making coke from it at all times pro-

Jan 1, 1923

By M. Sheffield

This paper presents a technique lor predicting the flow of oil, gas and water through a petroleum reservoir. Gravitational, viscous arid capillary lorces are considered, and all fluids are considered to be slightly compressible. Some theoretical work concerning the fluid flow in one-, two- and three-space dimensions is given along with example performance predictions in one- and two-space dimensions. INTRODUCTION Since the introduction of high speed computing equipment, one of the goals of reservoir engineering research has been to develop more accurate methods of describing fluid movement through underground reservoirs. Various mathematical methods have been developed or used by reservoir engineers to predict reservoir performance, 193-5,7,8 The work reported in this paper extends previously published work on three-phase fluid flow (1) by including a rigorous treatment of capillary forces and (2) by showing certain theoretical mathematical results proving that these equations can be approximated by certain numerical techniques and that a unique solution exists. DISCUSSION The method of predicting three-phase compressible fluid flow. in a reservoir can be summarized briefly by the following steps. 1. The reservoir, or a section of a reservoir, is characterized by a series of mesh points with varying rock and fluid properties simulated at each mesh point. 2. Three partial differential equations are written to describe the movement at any point in the reservoir of each of the three compressible fluids. All forces influencing movement are considered in the equations. 3. At each mesh point, the partial differential equations are replaced by a system of analogous difference equations. 4. A numerical technique is used to solve the resulting system of difference equations. Capillary forces have been included in two-phase flow calculations.1,4,8 The literature, however, does not contain examples of prediction techniques for three-phase flow that include capillary forces. Where capillary forces are considered, each of the three partial differential equations previously discussed has a different dependent variable, namely pressure in one of the three fluid phases. Therefore, three difference equations must be solved at each point in the reservoir. Where large systems of equations must be solved simultaneously, an engineer might question whether a unique solution to this system of equations actually exists and, if so, what numerical techniques may be used to obtain a good approximation to the solution. It is shown in the Appendix that a unique solution to the three-phase flow problem, as formulated, always exists. It is also shown that several methods may be used to obtain a good approximation to the solution. The partial differential equations and differenceequations used are shown in the Appendix. Matrix notation has been used in developing the mathematical results. Two sample problems were solved on a CDC 1604. They illustrate the type of problems that can be solved using a three-phase prediction technique. SAMPLE ONE-DIMENSIONAL RESERVOIR PERFORMANCE PREDICTION A hypothetical reservoir was studied to provide an example of a one-dimensional problem that can be solved. Of the several techniques available, the direct method of solution as shown in the Appendix was used. The reservoir section studied was a truncated, wedge-shaped section, 2,400 ft long, with a 6' dip. (A schematic is shown in Fig. 1.) This section was represented by 49 mesh points, uniformly spaced at 50-ft intervals. The upper end of the wedge was 2 ft wide, and the lower end was 6 ft wide. The section

Jan 1, 1970

By R. J. Wagner, F. F. Craig, H. G. Riley, J. D. Griffith

Peripheral water injection has been underway in the Sholem Alechem Fault Block "A" Unit, Stephens County, Okla., since 1955. In the engineering planning of the flood, it was recognized that maintenance of pressure in the large, dry gas caps was vitally necessary to prevent the loss of an estimated 27 million bbl of oil through saturation of the gas caps by the oil banks moving updip on the peripheral flood pattern. The development of an abundant, low-cost water supply and the rising cost of makeup-gas purchases indicated that gas-cap control by water injection was desirable from an economic standpoint, provided an eflective water barrier could be placed without premature water breakthrough into downdip oil producers. A laboratory model scaled to the existing reservoir conditions was comtructed to evaluate the feasibility of gas-cap water injection. Model studies indicated that (I) water injected at the edge of the gar-oil contact would form a continuous barrier between the oil and gas zones, and (2) water would advance uniformly downdip without segregation due to gravity effects provided a specified, minimum water-injection rate was maintained. The model test results also indicated that it was not necessary to fill the gas cap completely with water. Water injection at the edge of one of the gas caps was initiated in March, 1958, to field test gas-cap water injection. Water breakthrough occurred at a downstruc-ture producing well in April, 1959, after approximately 2.5 million bbl of water had been injected into the gas cap. This was the volume calculated to be required to form the barrier between the oil zone and gas cap. This performance indicates that prevention of oil encroachment into dry gas caps in a peripheral water flood by water injection at the gas-oil contact appears practical and that the model studies provided a valid prediction of field performance. INTRODUCTION The Sholem Alechem Fault Block "A" Sims Sand Unit was one of the fist major waterflood projects in Oklahoma to utilize a peripheral injection pattern. Design of control measures to minimize oil encroachment into the large crestal gas caps was one of the greatest single problems during engineering planning of this flood. Engineering studies indicated that saturation of the gas caps with oil displaced by the peripheral water flood could result in a loss of about 27 million bbl of oil, or over one-half the estimated waterflood recovery. This estimate was based on a residual oil saturation after water flooding of 35 per cent pore volume, compared to the negligible oil saturation initially in the gas caps. The Sholem Alechem Springer field, located in Stephens County, Okla., is an elongated anticline with structural dips varying from 400 to 1,000 ft/mile. The structure contains numerous faults, some of which are sealing. The portion of the field considered in this paper is Fault Block "A", which is the largest of the five major fault segments in the field. A map of the unit is shown on Fig. 1. The unit is bounded on the east and west by major sealing faults, on the north by a water-oil contact and to the south by a deterioration of sand development. Two domes, each having gas caps, exist in the unit and are separated by a north-south fault as shown in Fig. 1. The sands being flooded are the Sims sand members of the Springer series of early Pennsylvanian age. The Sims sands average over 100 ft in thickness in Fault Block "A" and have a porosity of approximately 19 per cent. Core permeabilities average 160 md, with interstitial water saturation of about 23 per cent pore volume. Three different zones can be correlated over most of the area. However, they are commingled in most of the producing wells. The two upper zones, designated as First and Second Sims, are the most important. Both the First and Second Sims have gas caps in the east dome, while only the First Sims has a gas cap in the west dome. These gas caps, whose limits are also shown on Fig. 1, initially occupied nearly 11 per cent of the total reservoir volume. The major concern of this paper is the control of the two gas caps in the First Sims sand. Fig. 2 is a cross section, to scale, across the east dome of this formation. Notable features are the relatively shallow dip, the deterioration of the First Sims sand on the south side of the gas cap and the water-oil contact on the northern edge. The formation dip at the gas-oil contact in this cross section is approximately 5".

By R. W. Smith, K. H. Lee

Bond type simulated closed-circuit grindability tests and batch grindability tests were run on six pure minerals plus a limestone and a taconite ore. The simulated closed-circuit tests were made at five different meshes of grind. The minerals tested varied widely in hardness and breakage pattern. For all simulated closed-circuit tests both Bond and Holmes work indices were calculated and compared. The Bond grindability testlm6 has been widely and quite successfully used for predictions of such items as ball mill power requirements and as an aid in plant comminution equipment selection. The test is interesting in that although run as a series of batch tests it is over-all a simulated closed-circuit test with a circulating load of 250%. The simulated closed-circuit feature is probably the primary reason for the notable success of the test. Perhaps the major criticism that can be brought against the test is that it is time consuming, since it normally takes a trained technician about an eight-hour shift to perform it.4 For many purposes this is an acceptable time requirement. However, if a grindability test is to be used for mill control purposes it should be performed in as short a time interval as possible, preferably under an hour. Sometimes in industry strictly batch tumbling mill tests are run and an attempt is made to correlate such batch tests with plant mill operation. Then an attempt is made to adjust operating tumbling mills based on data from the tests. The tests, however, frequently do not correlate well with operating data. The purpose of the present work was to explore some of the similarities and differences between a simulated closed-circui.t grindability test and a batch type test. Six different minerals plus a limestone and a taconite ore were tested in the experimentation. These materials varied widely in hardness, breakage characteristics, etc. Standard dry Bond grindability tests were mn on all materials at 48, 65, 100, 150 and 200 meshes of grind. Feed material was prepared by stage cmshing to -6 mesh. Initial feed volume was 700 cc. Care was taken to maintain the standard constant weight (about 20125 gm) and number of balls (283) during all the tests. Rotational speed was 70 rpm. Table I lists the materials studied along with pertinent data regarding the materials and Bond grindabilities obtained. In addition, dry batch tests were performed on all materials. These tests were made in the same mill as was used for the Bond tests. An identical ball charge and an identical feed volume were used. After rotating the mill for a predetermined number of revolutions at the same rotational speed as for the Bond test, the material was removed and separated from the ball charge. A screen analysis was performed on this product. Knowing the original size distribution of the feed and the size distribution of the product, it was possible to calculate the grindability or grams of a particular mesh produced per revolution of the mill. After the screen analysis of the product, the various fractions were recombined and placed back in the mill for further grinding. After grinding for additional revolutions of the mill the procedure was repeated. Thus, it was possible to obtain grindabilities for each material at a number of meshes of grind and for various revolutions of the mill. Grind-abilities obtained from batch tests are shown in Table 11. COMPARISON OF BOND AND BATCH GRINDABILITIES Figs. 1A through 1D show relationships between batch and Bond grindabilities. Figs. lA, lB, 1C and 1D show respectively graphs indicating the relationships for batch tests run for 100, 300, 500 and 700 revolutions of the mill. For a particular material on each graph, points are shown for 200, 150, 100, 65, and 48 meshes of grind except for several missing coarse meshes of grind for galena which did not fall conveniently on the figures. For each material and graph the point nearest the origin is for 200 mesh, the next for 150 mesh, the next for 100 mesh, etc. Considering Fig. lA, it is interesting to note that all relationships shown are essentially straight lines. There are, however, considerable differences

Jan 1, 1969

By Russell Dayton

THE metallurgical polarization microscope has been utilized in several researches in the last few years, thus attaining a fair degree of prominence, but little has been written in a manner suitable to a metallurgist concern-ing the theory of this instrument. In this investigation the theory was carefully studied, and the results are presented here in a detailed manner, yet as simply as possible. The theory is discussed with particular reference to the three chief functions of the instrument: (1) determination of anisotropy; (2) effect of strain; and (3) identification of inclusions. Each of these is investigated experimentally, with especial attention to the mechanism of producing any effect. Where possible, the discussion is supplemented by photomicrographs. The instrument used had numerous defects as a polarization microscope; these and their remedies are discussed. In the microscopic study of transparent mineral sections (chal-cography) the use of polarized light has aided tremendously in the identification of a mineral. The determination of strain in transparent substances (photoelasticity) by the use of polarized light has lately become a commercial process, used in testing finished glass articles. The success of the use of polarized light with opaque materials has not been so great. The magnitude of the effects obtained is much less than that of the corresponding effects with transparent materials, and the mechanical difficulties are much greater. Konigsberger,(1)? in 1909, was the first to apply polarized light to the microscopic study of

Jan 1, 1935

By G. L. F. Powell, L. M. Hogan

Samples of silver and Ag-O alloy, 0.12 wl pet, have been undercooled to a maximum of 250°C by melting in a slag of commercial soda-lime glass. Grain refinement occurred in undercooled silver samples whet the degree of undercooling exceeded a critical value which varied from 153° to 175°C, depending on the melting conditions. In under cooled Ag-0 samples, the grain structure was fine and equiaxed at degrees of undercooling larger than 50oC. The grain refinement in both silver and Ag-0 alloy samples was the result of recrystallization during or immediately following freezing. When the oxygen content was increased, the degree of undercooling at which recrys-tallization occurred decreased. INVESTIGATIONS of the grain structure of strongly undercooled melts of nickel and cobalt1-4 have revealed a change in room-temperature grain size as a function of undercooling. At large degrees of undercooling the grain size was fine, but samples undercooled by smaller amounts exhibited a much coarser grain structure. The reported undercooling at which this grain size transition occurred in nickel varied between 140° and 175'C undercooling. Walker1 attributed this grain size change to an enhanced nuclea-tion rate. Cavitation at a melt-solid interface was con sidered to generate a high-pressure wave. This, in turn, produced nucleation in the liquid as a result of an elevated freezing point increasing the undercooling in the melt. A similar grain size transition was observed in undercooled silver between 133° and 153°C undercooling.5 The grain size transition in undercooled silver was found to be dependent on oxygen con tent. More recently, the authors5 showed that a simila transition occurred in an undercooled Cu-O alloy, =0.08 pet, but not in oxygen-free copper undercooled more than 200°C. The transition was attributed to recrystallization of the solidified grains after freezing; the greater the degree of undercooling, the more complete the recrystallization. In view of this effect of oxygen content on grain size transition, additional undercooling experiments were carried out with silver. This paper reports the results of these studies on silver and Ag-O alloys undercooled more than 50°C EXPERIMENTAL 1) Materials. The silver was supplied by Matthey Garrett Pty., Ltd., as fine granulate, silver mini' mum 99.9 pet, and contained the trace impurities shown in Table I. The silver originated from two different refineries resulting in the difference in impurity content shown in Table I. However, the variation in composition had no discernible effect on the undercooling behavior. Samples of the silver were melted in an open-ended, vertical, cylindrical resistance furnace, wound with Kantha] wire, the temperature of which was adjusted by means of a variable transformer, 2) Melting and Undercooling. Bulk samples of silver were undercooled by preoxidation and removal of oxidized impurities in a glass slag, as previously described,5 but special precautions were necessary to allow comparison between oxygen-free silver and a Ag-O alloy. Samples free of oxygen were prepared by first melting weights of granulate varying from 200 to 400 g in clean vitreous silica crucibles in air for approximately 15 min. A sample was frozen and a complete glass cover formed over the top surface by adding granulated glass rod. The sample was then melted and frozen several times until no oxygen bubbles appeared in the glass slag. Subsequent thermal analysis indicated that the oxygen content was negligible. The glass acted as an efficient barrier to absorption of oxygen from the air. Ag-O alloys were prepared by melting silver in silica crucibles with only a partial cover of glass, so that the top surface of the melt was in contact with air. The silver was held molten in air for several hours at 1000° to 1050°C, in the expectation that the oxygen in solution would reach equilibrium with atmospheric oxygen. At T - 1000°C the equilibrium oxygen content was calculated as 0.12 wt pet O, using Sieverts law and Eq, [l], derived by Mizikar et a!.7 from the data of Sieverts and Hagenacker8 for 1 atm of oxygen:

Jan 1, 1970

By G. P. Gladis, R. H. Atkinson

Palladium has been used for jewelry for many years, particularly in conjunction with gold. This use increased in amount during the war, as palladium and gold were only moderately used for war purposes while demands for platinum and some of the other members of the platinum group were so great that their use in jewelry was prohibited. Palladium hardened with a small percentage of ruthenium has the necessary technical properties and appearance for good jewelry, and it is sufficiently rare to be desirable for luxury items—at least I00 times as rare as gold. Although both visual and spectro-photometric examination demonstrated that the color of Palladium was almost the same as that of platinum, a few jewelers found the surface of palladium, even after some polishing, rather dark in areas that had been repeatedly heated during the soldering necessary to assemble certain types of handmade ornaments. This phenomenon is not to be confused with the thin, bluish oxide film that can be produced by heating in air over the range 400' to 800°C., as that film is easily reduced by dipping in warm 5 per cent formic acid or in warm methanol. It was suspected that the difficulty arose from heating in atmospheres that were alternately oxidizing and reducing, as Wise and Vines1 had found that this opened the grain boundaries of palladium and palladium-silver alloys in the same manner as in pure silver, as reported by Martin and Parker.2 This damage is caused by the reaction between oxygen in solid solution in the metal, acquired when heated under oxidizing conditions, and hydrogen diffusing in from subsequent heating under reducing conditions; the steam cannot diffuse out and therefore builds up sufficient pressure to disrupt the metal near the surface. Copper and various other metals can be damaged similarly, but platinum is nearly immune; therefore the problem was new to the platinum jeweler. Sulphur in the fuel gas also can cause trouble but did not appear to be dominant in the present instance. Metallographic examination of both pure palladium and ruthenium-palladium showed that the usual torch using oxygen and city gas as normally operated did in fact cause the surface and subsurface damage that had been observed, and also disclosed that a reducing flame caused more damage than an oxidizing flame and was very damaging even in the absence of any intentional swing in atmosphere from oxidizing to reducing (Fig. 7); besides the surface damage, there was serious loss of ductility. A full explanation of the mechanism of attack is not evident at the moment, but may be allied to the attack that occurs on heating catalytically active metals in nonequilibrium atmospheres.

Jan 1, 1946

By Frederick L. Knouse

THE south border of Espirito Santo begins about 400 km. north of Rio de Janeiro and extends along the Atlantic Coast northward some 325 km. and inland 100 to 150 km. The area under consideration, where quartz crystal of strategic grades has been mined, extends from 19° to 21° and 30" south latitude; and from 40° to 41° and 30" west longitude. This includes the central part of Espirito Santo, chiefly south of the Rio Doce from the Atlantic ocean, and west across the border into Minas Gerais near the town of Aimores, in the municipalities of Aimores, Minas Gerais; Baixo Guandu, Santa Teresa, Santa Leopoldina, Colatina, Joao Neiva, Fundao and Domingo Martines, Espirito Santo (Fig. 1). During 1943 and the first half of 1944, this region accounted for approximately 3 to 5 per cent of the quartz crystal produced in Brazil. Shipments of crystal have been made chiefly by rail to Rio de Janeiro. This region is serviced by the E. F. Minas-Vitoria and E. F. Leopoldina to Rio de Janeiro through Vitoria; and by the E. F. Minas-Vitoria and E. F. Central do Brasil through Bello Horizonte, Minas Gerais to Rio de Janeiro. The major deposits are accessible from the railheads by dirt roads, some being 5 to 30 km. off the road, reached by trail. In 1943 and the first half of 1944, the bulk of the production was from inter mountain marshes and adjoining hillside alluvial placer deposits in the zone surrounding the town of Santa Teresa. Most of these deposits were formed from the erosion of pegmatites, quartz veins and pockets in the gneiss, with minor quantities produced from miarolitic cavity fillings in the granitic rock. EARLY OPERATIONS Mining of quartz crystal in this region began in 1928, and has been stimulated by the market demand for military uses. Before 1936 little attention was given to it, either in Espirito Santo or eastern Minas Gerais. From 1936 to 1941 the Japanese sent agents to various points of production or potential production to acquire quartz through purchase. They bought crystal as small as 10 grams. Since 1941 only the United States and Great Britain have received quartz from Brazil. The United States purchases crystals of loo grams and larger for strategic purposes. The first known discoveries were made either in the municipalities of Aimores, Minas Gerais, or in Baixo Guandu, or Domingos Martines, Espirito Santo. Marketable quartz crystal was first found either in the massive quartz replacement veins of the Victor Hugo mine in the municipality of Domingo Martines, or in the large cores of quartz in the pegmatites near Baixo Guandu, extending into Minas Gerais. PRODUCTION The production of quartz in Espirito Santo from 1936 through 1941 as recorded

Jan 1, 1946

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, 1944

By L. A. Delano

During 1916, the St. Joseph Lead Co. milled 2,505,670 tons of ore. This is a daily operating average of 7855 tons. The economic concentration of such a large tonnage necessarily requires a plant equipped with modern machinery and operated efficiently. The milling process used in producing this output has been a gradual development through the long period of years that the company has been in existence. HISTORICAL SUMMARY OF MILLING PRACTICE Ore was first mined at Bonne Terre, Mo., in 1864. The early milling practice was crude. It consisted of breaking the ore into small pieces by hand, pulverizing in a Blake crusher and a pair of Cornish rolls to approximately minus 6 mm., and jigging in the old-fashioned hand jigs. Only the coarse heavy galena was saved, the gangue being shoveled off and discarded. The output for the first year under this method was only 240 tons of pig lead. The first mill of the company was a combination of extensions and additions built from time to time as the mines developed. It was a museum of early milling machinery, such as jigs, percussion tables, buddies, dolly tubs, log washers, etc., following no definite flow sheet. The chats, or tailings, were hauled to waste dumps by mule and ox teams, as much as 500 tons per day being moved in this manner, until a railroad was built in 1880. This mill was burned in 1883, at which time the annual output had reached approximately 7300 tons of pig lead. A new mill of 500 tons capacity was designed and built by C. B. Parsons. This mill has been admirably described by H. S. Munroe.' The ore was crushed in Blake crushers, Cornish rolls, through 6-mm. screens, and treated by jigs of the Parsons type, percussion tables and log washers, or trunking machines, for cleaning the galena. The middlings were recrushed in rolls and treated on Harz jigs. The mill was operated without change, except later installing Gates crushers and en-

Jan 1, 1918