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Philip Argall, Denver Col. (communication to the Secretary): Dr. Raymond claims (Trans., xxiii., 560)) that my statement (p. 557) regarding the crystallization of iron "is beyond question incorrect." He says: "It is not even settled that vibration will crystallize iron under any conditions." While admitting that authorities differ on the possibility of cold crystallization of iron, I believe it is a settled and undisputed fact that vibration in the presence of heat will crystallize iron. Bloxam and Huntington say :* " Vibration assists 'in converting fibrous metal (iron) back into a crystalline state when heated, a lower temperature sufficing than in the absence of vibration." Mr. A. F. Hill, summing up a very exhaustive review upon the crystallization of iron and steel, pronounces against crystallization, but only at temperatures below 900' F. Mr. Howe, discussing ,the breakage of a 20-foot porter-bar with a crystalline fracture, suggests that it was attributable to heat, jointly with the jar. We see, then, that vibration of heated iron bars will induce crystallization and consequent change of structure. Referring to my statement, I wish to point out, that I was discussing the vibration of stamps arid should have said, "vibration under all such conditions," etc. That is, vibration attended with sharp blows, such as a stamp-stem is subjected to, will crystallize iron; yet I believe that intense vibration under any condition will

Jan 1, 1895

By Dewitt T. Ring

Lack of reliable detailed production figures for earlier years, together with the loose nomenclature in reference to producing horizons and the application of the term "field" without any definite meaning or restriction, has made it impossible to gather statistical data suitable for the Institute's form. In common with all other producing areas in the United States, Ohio has felt severely the economic ills of the entire industry during the past year. With overproduction, not only of crude but also of refined products, going on throughout the country, the price structure as a direct consequence has weakened on Ohio oils. Valuable crude is being sold at a big loss today because producers arc willing to, and do, sell more than the market can absorb. The axe hangs heavy over the heads of Ohio producers, and will until something constructive is done to keep supply in proportion to demand. This not only applies to Ohio but to the entire industry. Production of Pennsylvania grade in Ohio was under 50 per cent proration, which has been in effect since Oct. 1, 1937. Three price cuts since February have lowered the posted price from $1.70 to $1.18, a 30 per cent reduction; other grades were less drastically reduced. Pipeline storage facilities were limited; many producers were faced with the problem of providing their own storage or the risk of ruining their wells. If they wanted to pull and abandon wells, there was no market for junk equipment. Many employees have been cut to half time and in a number of instances their services entirely dispensed with. Summary of Production and Drilling Both oil and gas production in the state during 1938 showed a definite decline over the previous year. (A table showing production by years from 1876 through 1937 was published in Vol. 127 of the Transactions.) The total production of crude oil in the state for 1938 was 3,357,914 bbl., as compared with 3,654,000 bbl. in 1937, a decrease of 7.1 per cent. At

Jan 1, 1939

By Dewitt T. Ring

Lack of reliable detailed production figures for earlier years, together with the loose nomenclature in reference to producing horizons and the application of the term "field" without any definite meaning or restriction, has made it impossible to gather statistical data suitable for the Institute's form. In common with all other producing areas in the United States, Ohio has felt severely the economic ills of the entire industry during the past year. With overproduction, not only of crude but also of refined products, going on throughout the country, the price structure as a direct consequence has weakened on Ohio oils. Valuable crude is being sold at a big loss today because producers arc willing to, and do, sell more than the market can absorb. The axe hangs heavy over the heads of Ohio producers, and will until something constructive is done to keep supply in proportion to demand. This not only applies to Ohio but to the entire industry. Production of Pennsylvania grade in Ohio was under 50 per cent proration, which has been in effect since Oct. 1, 1937. Three price cuts since February have lowered the posted price from $1.70 to $1.18, a 30 per cent reduction; other grades were less drastically reduced. Pipeline storage facilities were limited; many producers were faced with the problem of providing their own storage or the risk of ruining their wells. If they wanted to pull and abandon wells, there was no market for junk equipment. Many employees have been cut to half time and in a number of instances their services entirely dispensed with. Summary of Production and Drilling Both oil and gas production in the state during 1938 showed a definite decline over the previous year. (A table showing production by years from 1876 through 1937 was published in Vol. 127 of the Transactions.) The total production of crude oil in the state for 1938 was 3,357,914 bbl., as compared with 3,654,000 bbl. in 1937, a decrease of 7.1 per cent. At

Jan 1, 1939

By W. A. Tiller, J. P. McHugh

HE majority of liquidus and solidus surfaces in phase diagrams have been determined by the conventional cooling- and heating-curve techniques.' These techniques have two main shortcomings: 1) the solidus may be in considerable error due to the difficulty involved in completely homogenizing the solid and 2) the determination of liquidus and solidus in more than a two-component system does not enable one to determine tie-lines connecting the specific equilibrium solid and liquid compositions. However, in a recent paper by one of the authors,' a method was suggested whereby the liquidus and solidus surfaces plus tie-lines in an n-component system may be determined. This method utilizes a controlled solidification technique and assumes that interface equilibrium exists during freezing. The present work was undertaken with a twofold purpose; first, to determine the liquidus and solidus lines in the pseudo-binary system Bi2Te3-Bi2Se3 by heating- and cooling-curve techniques and, second, to determine the partition coefficients of Te and Se in the BizTe3-,Sex system by controlled solidifica- tion techniques. The two sets of results can be compared to test the accuracy of the controlled solidification method. EXPERIMENTAL I—The starting materials for this study were 997999 pct Bi, Te, and Se, obtained from the American Smelting and Refining Co. The compounds BizTe, and Bi2Se3 were each prepared by melting together stoichiometric amounts of the elements, followed by twelve zone-refining passes. This produced homogeneous bars of the compounds for use in the phase-diagram studies. The apparatus used to obtain heating and cooling curves is illustrated schematically in Fig. 1. The alloy samples were located in a graphite crucible placed in a stainless steel canister. The canister was supported in a heavily lagged pit furnace by a device which oscillated the canister about its vertical axis at a frequency of about 3 cycles per sec during heating and cooling-curve runs. The graphite crucible was designed to minimize the thermal coupling of the sample to the furnace. A thin graphite sleeve separated the alloy sample from the stainless steel tube that housed the thermo-

Jan 1, 1960

By AIME AIME

AT a joint meeting of the Tulsa Geological Society and the Mid-Continent Section of the A; I. M. E., held at Tulsa on March 21, the history of unit development in the Kettle- man Hills field was discussed. Robert C. Patterson? Super- visor for the U. S. Geological Survey at Taft, Calif., was the speaker. An abstract of some of his remarks follows: On July 1, 1923, curtailment agreement for two years was made between the operators of North Dome Kettleman and the U. S. Department of the Interior. In this it was agreed to consider a plan of unit development, or other cooperate method of developing the structure. As a result, Kettleman North Dome Association was incorporated in December, 1930, as a non-profit cooperative corporation under the laws of California. Approved in January, 1931, by California Oil and Gas Supervisor and by Secretary of Interior. On Feb. 10, 1931, it became an active organization through election of executive officers and eleven- directors. General manager chosen. Association started to function April 1, 1931. Assumed control of 10,800 acres of proved and semi-proved land, as shown in Table 1.

Jan 1, 1932

By S. LeFevre

THE solution of the housing and sanitation problem in mining communities, keeping in view both economic and humanitarian aspects, demands the best thought of the management of such enterprises. Upon the solution depend the health and comfort of the employee and his family, and as a consequence his contentment and efficiency. The following description covers briefly the methods installed for Witherbee, Sherman & Co. The operation of the system has been for about two years under the direct supervision of T. A. Hammond, Land Agent, and I am indebted to him for a compilation of the results.

Jan 2, 1915

By Benny J. Nelson

AS a part of the fundamental research program of Aluminum Research Laboratories, some data were obtained on the ternary system Mg-Al-Mn. As very little information on the magnesium corner of this diagram has heretofore been published, it seems desirable to make available the values found for the liquidus and solidus surfaces of this system. Procedure The settling procedure was used for the determination of the liquidus compositions. Metallo-graphic examination of quenched samples, and stress-rupture upon incipient melting, were used for the solidus determinations. The settling procedure has been described in a previous paper.' Briefly, this method involved saturating the alloy with manganese at a temperature substantially above that at which the sohbility was to be determined, then cooling the melt to the latter temperature, and holding it at that temperature for a substantial period of time. Samples for analysis .were carefully ladled from the upper portion of the melt at hourly intervals during the holding period. After the ladling of each sample, the melt was stirred to redistribute some of the manganese that had already settled, because it appeared that when the latter particles of manganese again settled, they aided in carrying down more of the manganese and thus hastened the attainment of equilibrium. The melts were prepared and held in a No. 8 Tercod crucible holding approximately 4 lb of metal. The manganese was added either in the form of a prealloyed ingot (Dow M) containing about 1.5 pct Mn or by the use of a flux (Dow 250) containing manganese chloride. In calculating the flux additions, it was assumed that the manganese introduced would be equal to 22 pct of the total weight of the flux. Temperatures were measured with an iron-constantan thermocouple enclosed in a seamless steel tube, the lower end of which was welded shut. This protection tube also served as a stirring rod. The samples ladled from the upper portions of the melts at the various intervals were analyzed for aluminum, manganese, and iron. When making the alloys which were to be used for the determination of the solidus, 2½ in. diam tilt mold ingots were cast, scalped to 2.0 in. in diam, and extruded into ? in. diam wire. The principal impurities in the melts for this investigation were iron and silicon; their total not exceeding 0.03 pct. Portions of the wire, approximately 2 in. in length, were enclosed in stainless steel capsules for protection from the atmosphere. Bundles of these capsules, with a dummy capsule containing an iron-constantan thermocouple, were heated inside a large steel block (acting as a heat reservoir) in a closed circulating-air type electric furnace. At ap- propriate times, the capsules were removed and quenched in water. The wires were examined metallographically to determine the temperature of initial melting. Short times at temperature were used at the beginning for wire specimens of all alloys to obtain quickly the approximate temperatures at which melting could be first observed. When approximate solidus temperatures had thus been determined, equilibrium heating was attempted. This equilibrium heating consisted of an 8 or 16 hr period at a temperature, about 50 °F below the lowest temperature at which melting occurred when short heating cycles were used, followed by further heating for 1 hr periods at consecutive 10" higher temperatures. The theory for the method of stress-rupture at incipient melting has been well covereda and its limitations are recognized. Thus, if the interfacial tensions are such that the first minute quantity of liquid is "bunched up" at the grain boundary junctions instead of spreading out along the grain boundaries,³ temperatures higher than the solidus are required before melting will be manifested by rupture of the specimen. This point will be elaborated later. Specimens of the wires with a reduced section (approximately 1/16 in. diam) were suspended vertically in a tubular furnace. The setup used is shown in Fig. 1. The clamp holding the specimen was made from alumel thermocouple wire and the thermocouple was thus completed across the specimen by attaching a chrome1 wire to its lower end. Temperatures were read from a Speedomax recorder used in conjunction with a calibrated thermocouple. The small weight attached to the specimen and a vibrator attached to the furnace tube, to aid in distributing the molten constituent along the grain boundaries, were used to bring about rupture at a temperature closely approximating the solidus. The specimens were heated at a rate of about 5°C per min. The rupture of the specimens was indicated both by sound and by the action of the recorder. An argon atmosphere containing a small amount of SO² was used for protection of the specimen. The assembly was taken out of the furnace immediately following rupture and the specimen removed. Some of the broken specimens were examined metallographically and will be referred to later. Results and Discussion Fig. 2 shows a set of typical time-composition curves for liquid samples of the Mg-Al-Mn alloys used for the settling tests. The data as presented

Jan 1, 1952

By H. H. Rachford, D. S. Howard

In the withdrawal of fluids from tilted aquifers it is of value to be able to predict pressure patterns during the course of the pressure decline. As an example of this, in the displacement of fluids from oil reservoirs being produced by water-drive, prediction of the reservoir pressure is an important factor in fixing production rate. The prediction of pressure patterns in the depletion of an inclined aquifer has conventionally been made by solving the well known flow equations for the pressure Patterns in a horizontal aquifer, and correcting these patterm for the pressure difference due to the hydrostatic head associated with the vertical distance between a point in the horizontal aquifer and the corresponding point in the tilted aquifer. Inasmuch as the equation describing flow in tilted strata is different from that for horizontal flow. there was question as to the validity of the simple corrective procedure current1y in use. To examine the magnitude of error made using this procedure, an inclined aquifer was chosen for which the error was expected to he large, and the equation for flow in this tilted stratum was solved numerically. The results of the conventional procedure of correcting the solution of the equation for horizontal flow was compared with the solution of the correct equation by studying the difference between predicted pressures by the two methods. Three forms of the hydrostatic head correction were studied. The results for all three forms of the head correction are similar. The error in the approximate solution is quite dependent on the position of the horizontal aquifer with respect to the inclined one. The error is greatest at the producing end ad increases with amount of fluid withdrawn. The magnitude of the errors is not large if a good choice is made for the position of the horizontal datum. The most satisfactory position for the datum in all cases is near or slightly about the mid-point of the inclined stratum. Use of the best approximate method studied with the best datum tested yielded predicted pressures in error no greater than 7 psi. INTRODUCTION The movement of water by expansion from an aquifer to displace fluids from a contiguous oil reservoir was first recognized over 20 years ago.9 Since that time much work has been done to relate this mechanism to reservoir behavior mathematically. The result of this effort on the part of many workers has led to an understanding of underground fluid movement which has enabled us to follow and predict the behavior of the water-drive reservoir. One reason that good progress has been made in the application of mathematics to the study of pressure patterns and water movements in aquifers has been that the differential equation which describes this process is of a relatively simple form. The equation for the isothermal, horizontal, viscous flow of water through homogeneous sandstone is identical with that for the diffusion of heat through homogeneous solids, and this equation and means of obtaining solutions for it with many types of boundary conditions have been studied extensively. That this work has been highly successful is clearly emphasized by the large number of solutions developed for problems of interest both by methods of formal mathemat-

Jan 1, 1957

By R. Adair, W. R. Hudspeth, W. T. McDaniel

D. C. Ralston (U. S. Bureau of Mines, Washington, D. C.)—Flake mica can be beneficiated by a wider variety of methods than almost any known mineral. However, most of these methods are not recorded. It is therefore a pleasure to find a written record of another application of a new method of beneficiation. The fact that the Humphries spiral gives a concentrate containing the mica flake mixed with the slime and small grit has forced a further separation by screening, in which the finest of the flake will pass through. Fine flake has its uses and if mixed with slimes or clay is recoverable reliably only by flotation. This loss must be charged against the spiral. On the other hand, the new muscovite mica paper recently brought out by General Electric Co., can be made only with grit free flake larger than 50 mesh. It is of interest to learn from the authors whether the washing of the flake on a 50 mesh screen can take the grit content below 1 pct, to meet this new demand. Must another degritting process be used on the flake, like electrostatic treatment of the dried material? H. D. Snedden (The Humphreys Investment Co., Denver)—When recovering mica in the spiral, gangue particles coarser than 16 mesh can be rejected more readily when operating at a high pulp density (35 pct solids) or a low volume rate (—15 gpm). A launder screen as used by Lehigh Coal Co. has proved very satisfactory to partially dewater the mica concentrate and to reject any gangue slimes it may contain. Under certain conditions mica cleaning in the spiral can be improved by reagentizing the spiral feed, the object being to insure wetting of the gangue minerals and to agglomerate or prevent wetting of the mica particles. R. B. Adair (authors' reply)—The grit content of the mica recovered on Humphreys Spirals varies with the fineness of the launder screen used to clean the mica product. Normal practice has been the use of 80 mesh screen, which will produce a mica product of acceptable grit content for most purposes. By using a 50 mesh screen, and increasing the screen area per ton of feed, it is felt by the authors that a mica of 99 pct plus purity could be obtained. This statement would hold only in the case of mica feed which was well de-laminated, and free from "clay balls," (semikaclinized feldspar), which tends to follow the mica through the process.

Jan 1, 1952

By P. D. I. Honeyman, P. A. Faust

At the Miami plant of the International Smelting Co., Inspiration, Ariz., there are four reverberatory furnaces, all 120 ft. long. At present only one of these furnaces is in operation. It is operated as a wet-charge furnace, the charge being distributed for about 65 ft. down the furnace length. Usually this charge contains about 12 per cent moisture and runs 25 per cent sulfur, of which there is eliminated in the furnace from 25 to 30 per cent. The furnace is oil-fired, the fuel being burned in a battery of Cananea-type, low-pressure burners. The flame is kept short and conditions so adjusted as to obtain complete combustion within the furnace. The average furnace draft, taken through the verb arch, amounts to only 0.02 in. of H2O. Draft is purposely kept low to cut down infiltration through the flues and boiler settings, and control dampers are regulated to maintain this uniform condition throughout the charging as well as the smelting period. Hot gases discharge from the furnace uptake through a common header flue to the waste-heat boilers. The general layout and dimensions of the plant are shown in Fig. 1. Four Stirling boilers, two of class M-26 (713 hp.) and two class M-31 (850 hp.), serve the furnace. Three usually are sufficient to take care of normal operation, the fourth boiler being used as a spare when necessary. The distribution of hot gases to the various boilers is regulated by the dampers in the boiler exit flues. Normally the boilers closest to the furnace uptake would evaporate more water than do those farther away, but dampers are regulated so as to distribute fairly well the load between the several boilers. Steam from the waste-heat plant is delivered to the adjoining power house of the Inspiration company, where it is used both in the Nordberg blowing engines and for electrical generation. Steam pressures and temperatures recorded are those in the main power-plant header and are thus inclusive of all losses in about 500 ft. of 10-in. line. Steam for smelter heating and auxiliary use is taken from the main waste-heat header, is reduced to 125 lb. and distributed through separate lines. Boiler feed water is supplied by the power plant and consists of returned condensate, augmented to a large extent by make-up water

Jan 1, 1934

By M. J. Sinnott, J. C. Tobin

A technique for collecting and analyzing the small quantities of gases desorbed on heating metal powders has been developed. The gases collected from copper powders of various types of manufacture have been analyzed and found to contain H2O, CO2, and SO2. The quantities of gas evolved vary from 0.05 to 1.0 milliliter, under standard con-ditons of temperature and pressure, per gram of powder. The source of the gas has been traced to surface films on the powder. IN the powder-metal industry it is recognized that the presence of gases in the powders affects the processing and resulting properties of the sintered product. Several sources for these gases are possible; namely, chemical reactions with the sintering atmospheres, inclusion. of gases during compacting, dissolved gases in the metal powder, and sorbed gases on the metal-,powder surfaces.1, 2, 3 Since the quantities of the gases are relatively small, no direct attempt has been made to collect and analyze them nor to isolate their source. The work that has been done has been concerned with the dimensional stability of the product., its porosity, density, or mechanical and physical properties. Conclusions are drawn on the basis of studies of this type as to the probable effect of gases on these properties. 4, 5, 0 In the present investigation an attempt has been made to obtain quantitative data on the analysis and quantities of gases associated with copper powders manufactured in different ways. Apparatus was constructed to collect gases evolved from loosely packed powder samples on heating to various temperatures under a reduced pressure of helium. The powders were outgassed thoroughly in a vacuum prior to starting the collection operation in order to eliminate mechanically entrapped gases and to prevent the possible reaction of the powder with these gases. Experimental Procedures Materials—The major portion of the investigation was carried out on a single heat of water-atomized, oxygen-free, high-conductivity copper. A relatively coarse fraction of this powder, 20 to 100 mesh, was tested as a mixed powder and as various graded size fractions. The microstructure of this powder showed equiaxed grains and was clean and free from oxides and oxide eutectic. The particle size, as determined

Jan 1, 1959

By J. L. Bray, S. T. Ross

The paper provides electrometallurgical data on the problem of germanium removal from zinc sulphate solutions. Germanium traces have caused much concern to the zinc refiner. Confirmatory evidence of interaction between germanium and cadmium is presented. Statistical analysis of data expands its significance and enhances its value. Further research is outlined. THE literature contains many references to the effects of trace amounts of germanium in the production of electrolytic zinc. One of the authors had experience with this troublesome element as early as 1917 at Trail, B. C. In 1929, Tainton and Clayton' reported that concentrations of as little as one part per million of germanium were sufficient to cause serious losses in current efficiency. Liddell2 reported that trace amounts of germanium cause marked lowering of the hydrogen overvoltage of electrolytic zinc cells, so that commercial production was impaired. Bray3 recorded the history of germanium in relation to electrolytic zinc production, noting that concentrations below 10 ppm have been found to yield low current efficiencies and copious hydrogen evolution. Koehler' stated that germanium "when present to the extent of a small fraction of one part per million per liter, causes serious evolution of hydrogen with a corresponding reduction in current efficiency." Recently, however, S. W. Ross" reported, from Risdon, Tasmania, that "in the course of leaching . .. dissolved traces of germanium... if not removed almost completely ... increase the reversion of cadmium during the filtration of the copper-cadmium precipitate and reduce the current efficiency during subsequent analysis." The copper-cadmium precipitate referred to is the residue from the zinc-dusting purification of zinc sulphate leach solutions. In the face of such conflicting testimony and with the increasing industrial importance of pure germanium and zinc it was decided to investigate the relationship between cadmium and germanium. Furthermore, other work by the authors showed certain discrepancies to exist in the theories of Tainton, et al. In the laboratory, without marked efficiency decreases, the authors have deposited zinc successfully from solutions containing as high as 1 g per liter of germanium. This could be done only when there was no cadmium present. Preliminary investigations of the suspected rela- tionships were carried out by means of emission spectrographic analysis using a beryllium internal standard. Several solutions containing 100 g per liter of zinc, as zinc sulphate, and 1 g per liter of cadmium, as cadmium chloride, were prepared. These concentrations were on the order of those obtained during a commercial low-acid leaching process. Varying concentrations of germanium were added to these solutions so that the range of 0.0000 to 0.5000 g per liter of germanium was covered. A 250 ml sample of each solution was agitated with 2.5 g of zinc dust for 30 min, filtered, and the filtrates were examined spectroscopically. Qualitative evidences of cadmium traces were found in those filtrates which originally contained above 10 ppm of germanium. Reliability of the analytical method did not permit quantitative investigations since cad-Table I. Current Efficiencies Obtained at 0.0000 and 1.5000 G per Liter Cadmium Concentrations Ge Concentrastion,* Cd Concentration,* EtBclenoy, G per Liter G per Llter Pot 0.0000 0.0000 84.270 0.0010 0.0000 94.849 0.0050 0.0000 92.649 0.0075 0.0000 94.039 0.0100 0.0000 96.084 0.0000 1.5000 93.460 0.0010 1.5000 95.158 0.0050 1.5000 92.148 0.0075 1.5000 91.260 0.0100 1.5000 84.546 • Cd and Ge concentrations shown are those existing before zinc-dust purification. mium determination in the concentrations present in zinc-dusted solutions lacks sufficient sensitivity for reproducible results. As a consequence of the inability of the investigators to obtain acceptable results through direct quantitative analysis, an indirect approach was devised. This indirect method involved a study of the current efficiency, in a model zinc cell, as a function of the concentrations of cadmium and germanium. Variables such as cell temperature, voltage, current density, anode spacing, relative electrode area, degree of agitation, cathode preparation technique, time, acid concentration, and solution volume were held constant. Fig. 1 shows the cell used. The current was fur-

Jan 1, 1952

By Donald Cummings

MEASURES appropriate for the control of the silicosis hazard in mining cannot be formulated precisely, but sufficient knowledge1-19 has accumu-lated during the past quarter century to permit the suggestion of useful, though partly empirical, rules for its alleviation. The industrial hygienist today recognizes that the peril incurred by the inhalation of harmful dust is a function of two variable factors-the degree of harmful exposure and the specific susceptibility of the exposed individual to pulmonary injury. Con-trol of the danger arising out of prolonged contact with pernicious air-borne particulate matter is consequently best exercised by influencing both of these recognized variables. Obviously the problem has two broad aspects-one, medical; the other within the province of the engineer.

Jan 1, 1938

Flexibility is the keynote in designing modern exploration drills that and mobility. Add to the flexibility of individual drills the wide range of models, and the man looking for a drill has ample choice today. Weight? Choose from models as light as 50 lb or as heavy as 10,000 lb. Hole capacity? From less than 1 in. for smallest core drills to 20 in. or more for auger types. Transportation? The lightest go by packsack (in fact, that is one trade name) ; others are designed to go by Jeep, truck, on skids or are built on light trailers. Power? Select air power, gasoline or diesel engine, electric motor, or use a power take-off from the vehicle on which the drill is mounted. Drill bits offer almost as much variety as the drilling machines themselves. Many drills are suitable for a variety of uses, and often adapt to several types of bits with ease. Some of the types available are: diamond core, diamond reaming, rotary, auger, shot, and special soil sampling tools.

Oct 1, 1955

By John M. Bostwick

Bitumen is a general term for a group of materials composed of mixtures of hydrocarbons that are fusible and soluble in carbon disulfide. Included in the group are petroleum, asphalts, asphaltites, and mineral waxes. Asphalt is a dark-colored, cementitious solid or semisolid, which generally softens on heating and resumes a more viscous or solid state when cooled (personal communication). It is found in native form in fissures and pore spaces in rocks and as lakes. It is also obtained from the residues produced in petroleum refining. Asphaltites are black, naturally occurring solid bitumens. They are generally shiny and break with a conchoidal fracture. Common asphaltites are gilsonite (uintahite), grahamite, and glance pitch. Mineral waxes are solid or semisolid, relatively nonvolatile bitumens of various colors, having an unctuous feel and waxy luster. Of the native waxes, ozokerite is the best known. Montan wax is also classed as a natural wax, although it never occurs in the pure state and must be extracted from lignite or cannel coal (Ladoo, 1920). Mineral waxes may also be obtained by pyroprocessing of petroleum, lignite, and peat. Pyrobitumens are dark-colored, solid hydro- carbons that are infusible and relatively insoluble in carbon disulfide. They are so-called because they will yield liquid and gaseous hydrocarbons only when heated. Asphaltic pyrobitumens are defined as "substantially free of oxygenated bodies" and include wurtzilite (elaterite), albertite, and impsonite (Thrush, 1968). Nonasphaltic pyrobitumens contain oxygenated bodies; examples are coal and peat. The nonasphaltic type will not be discussed further. Petroleum Asphalts Asphalts refined from crude petroleum have almost completely replaced the native types. Refineries can produce asphalts in every desirable grade more economically and in greater quantity than the native types and with a variety of properties that meet the requirements of the various manufacturers using them. For all practical purposes, it is estimated that more than 95% of the asphalts consumed in the United States are refined from crude petroleum (private communication).

Jan 1, 1975

By W. E. Wrather

DURING the war the mineral industry, and metal mining in particular, extended itself more than any other to attain the limit of its productive capacity. Likewise, probably no other industry went quite so far toward jeop¬ardizing its own economic future through depletion of material reserves. Once we looked to Europe for most of the manufactured goods we needed. Our own limited mineral requirements were easily supplied from mines near the Eastern seaboard. With expansion and industrialization, our mineral needs increased in proportion, and the centers of mining activity moved westward to Michigan, Wisconsin, Minnesota, and the Tri-State district, where seemingly inexhaustible high-grade deposits of iron, copper, lead, and zinc ores were opened and rapidly developed.

Jan 1, 1946

By Lawrence F. Schubert

Instrumentation is not a stranger to the minerals processing industry. In fact, very few plants now exist that haven't to one extent or another adapted operations to instrumentation. But with the rapid growth of such controls has come the need for effective departments composed of men trained to maintain and repair the instruments; here is where many firms fall short. The importance of the role an instrument department should play is underscored by the omnipotent effects which instruments often exert over an operation. Reserve Mining Co. is an example: while instrumentation at this taconite plant represents approximately 2% of the process equipment cost, a breakdown of instruments may result in the ineffective use (or complete shut-down) of the other 98% of plant investment.

Jan 7, 1966

By K. A. Svanstrom, W. R. Opie

Problems associated with deposition of titanium infused chloride baths using TiCl4 as a feed material are reviewed. A potentially workable cell design using Alumdum diaphragms is discussed. Problems inherent to diaphragm-type cells are emphasized and experiments described which led to the development of a cell without a diaphragm. INVESTIGATORS assigned the problem of developing a commercial electrolytic process for making titanium metal have found that they are faced with the difficulty of overtaking rapidly improving magnesium and -sodium reduction processes. The ultimate goal must be a simple process that can be conducted with low-cost raw materials in equipment that is inexpensive to build and operate. This paper deals with some work of a preliminary nature conducted by personnel of the Research Laboratories, National Lead Co., Titanium Division. Many others have reported on the general subject of depositing titanium from fused salt electrolytes. A partial bibliography is attached. PRIMARY CONCEPTS Anyone attempting to deposit titanium metal from fused chloride electrolytes using TiC14 as a source material is faced with at least the following problems: 1) Getting the titanium into solution in the bath. 2) Controlling oxidation and reduction reactions associated with multiple valency of titanium, which result in low electrical efficiency. a) Prevention of dichloride oxidizing to trichloride and trichloride to tetrachloride at the anode. b) Prevention of trichloride from being reduced only to dichloride at the cathode. 3) Prevention of metal formation away from the cathode thru disproportionation of titanium dichloride to satisfy the equilibrium. 3 TiCl2 == 2 TiCl3 Ti [I] 4) Protection of reduced chlorides in the bath from reaction with oxygen from the bath container or air. 5) Removing from the bath the deposited metal formed without allowing it to become contaminated with oxygen or nitrogen. 6) Selecting cell materials of construction which will not contaminate the metal product or cause cell inefficiencies. EARLY EXPERIMENTS The initial attempts made to electrodeposit titanium from fused chloride baths using TiCl4 as a source material indicated that TiCl4 was essentially insoluble in molten chlorides of alkali and alkaline earth metals. If, however, the TiCl4 was introduced close to a nickel cathode some metal could be formed and appreciable quantities of reduced chlorides would be present. These reduced chlorides reacted with any oxygen present in the atmosphere above the bath and would also diffuse quickly to the anode (graphite) where they would react with chlorine and be evolved as TiCl4. The net electrolytic efficiency of such a cell is essentially nil. The TiCl4 evolves from the anode at almost the same rate that it is introduced in the vicinity of the cathode although a small amount of titanium metal can be formed on the walls of the cathodic pipe. It becomes apparent from the operation of such a cell that: metal can be deposited on the cathode, although of small particle size and a nonadherent nature, and when reduced chlorides are present in the electrolyte, TiCl4 can be absorbed, probably by the following reactions: TiCl4 + TiC12 - 2 TiCl3 [21 2 TiCl3 + 2 faradays - 2 TiC12 + C12 [31 DIAPHRAGM CELLS These facts encouraged the development of cells containing diaphragms to prevent migration of reduced chlorides from the cathode area to the anode. Small-scale cells for process development are described by Alpert, Schultz, and Sullivan.20 A larger brick-lined cell incorporating internal heating by passing ac through the bath is shown in

Jan 1, 1960

By K. A. Gschneidner, O. D. McMasters, T. J. O’Keefe

X-ray diffraction, differential thermal, ad rnetallo-graphic methods were used to establish the Dy-Pb Phase diagram. Lead additions lower the 1377°C transformation temperature of dysprosium to 1360°C leading to an inverted peritectic reaction. The 327°C melting point of lead is lowered by dysprosium additions to about 326°C yielding a eutectic reaction. A second eutectic reaction occurs at 13.3 at. pct Pb and 1200°C. The dysprosium-richest intermetallic compound DysPb3 melts congruently at 1695°C and crystallizes in the hexagonal Mn5Si3 (D8,) type structure. The peritectic decomposition temperatures for the remaining compounds are Dy5Pb, at 1555C, DyPb2 at 955C, and DyPb3 at 880°C. A fifth compound near the DyPb stoichiometry exists over a 310°C temperature range decomposing at 1130°C by means of an inverted peritectic reaction and melting incongruently at 1440°C. The crystal structures of the compounds are discussed. A systematic study of the rare earth-lead alloy systems is underway in an effort to supply information concerning the alloying behavior of the rare earth metals. The Dy-Pb phase diagram is the fourth system to be investigated in this study. The Yb-Pb,1 Y-Pb,2 and Eu-Pb 3 diagrams have been published recently. Utilization of the rare earth series of metals as a research tool in this manner should yield a better understanding of alloy formation. EXPERIMENTAL PROCEDURE Materials. The lead used in this investigation was obtained from Cominco Products, Inc., and was specified to be 99.99 pct pure. The dysprosium was prepared in this Laboratory by the calcium reduction of the fluoride followed by distillation of the dysprosium. The major impurities in the dysprosium in ppm are: A1 (<40), Ca (400), Er (<50), Gd (<200), Ho (<200), Mg (<50), Si (30), Ta (400), Tb (<100), Y (<50), 0 (651, H (15), N (not detected), F (430), C (35). Alloy Preparation. Most of the alloys were prepared by melting weighed amounts of dysprosium and lead in sealed tantalum crucibles. The tantalum crucibles were sealed by are-welding in a He-Ar atmosphere welding chamber. Thus the alloys are in contact with He-Ar at about 1 atm pressure. Homogenization was achieved by holding them in the liquid state for about 1 hr, cooling, inverting the crucibles, remelting, and repeating the process at least twice. Since these alloys were prepared in sealed tantalum crucibles, chemical analysis for final composition was thought to be unnecessary. No detectable reaction of these alloys with the tantalum crucible was observed by metallographic examination. Metallographic evidence was also used to confirm the homogeneity of some of the alloys prepared in this manner. The compositions of a few alloys, which were prepared by nonconsum-able are-melting, were corrected for the small weight losses involved by assuming that the weight loss is due to vaporization of lead. The specimens obtained from the alloy samples were prepared under a dry-argon atmosphere because they were rapidly attacked by air and moisture. Thermal Analysis. Differential thermal analysis methods were used to determine the liquidus curves and reaction horizontals of the system. Both Pt vs Pt + 13 pct Rh and W + 5 pct Re vs W + 26 pct Re thermocouples were used to measure the temperature. An X- Y recorder was used to record the specimen temperature and differential electromotive force between the specimen and molybdenum standard. The arrest temperatures were measured potentiometri-cally. The accuracy limits (* values) associated with the reaction temperatures obtained by this method were estimated on the basis of both the reproducibility of the particular temperature value and the accuracy of the thermocouple at a given temperature. Liquidus temperatures were obtained from cooling arrest data while both heating and cooling arrest data were used to establish the horizontals of the diagram. Heat treatments during the thermal analyses of the alloys between 40 and 70 at. pct Pb were necessary in order to approach equilibrium conditions. The samples were held at temperatures between the various peritectic horizontals for l to 2 hr before the thermal analyses were continued. The entire range of compositions was investigated at the expense of a minimum amount of materials by adding appropriate amounts of lead to master alloys. More than sixty alloys were analyzed by this differential thermal method and for each alloy the results given herein are taken from two or three heating and cooling cycles. X-Ray and Metallographic Methods. Slice specimens for metallography and powder specimens for X-ray diffraction were prepared from rod-shaped samples which had been melted in sealed 0.62 5-cm-diam tantalum crucibles. The specimens were heat-treated in sealed tantalum crucibles which were protected by sealing them in argon-filled quartz ampules. Quenching was accomplished by breaking the ampules in ice water after heat treatment. X-ray powder specimens were sealed in 0.3-mm-diam glass capillaries under a dry-argon atmosphere. Copper, iron, and chromium radiation were used to obtain the powder patterns for these alloys. More than 150 powder patterns were obtained for specimens of various compositions and heat treatments. Included in these were several patterns for specimens which had purposely been oxidized. Patterns from specimens which had been accidentally exposed

Jan 1, 1969

By C. S. Smith, L. H. Beck

KNOWLEDGE of the Cu-Zn constitution diagram was critically examined in 1944 by G. V. Ray-nor,1 who suggested the diagram reproduced in Fig. 1 as the best evaluation of available data. No pertinent work on the constitution has been published since that time, although a number of authors have discussed transformation kinetics and theory. Despite the large amount of work that has been done on the constitution of these industrially important and scientifically interesting alloys, minor uncertainties still exist. For example, it is still not possible to say definitely whether a two-phase region exists between the ordered and disordered forms of the 8 phase. A careful re-examination of the phase boundaries in this part of the diagram was therefore undertaken. Two methods were selected for the new investigation—quantitative metallography for the higher temperatures and precision lattice parameter measurement for lower temperatures. Because of the relatively narrow two-phase regions flanking the ß phase in these alloys, quantitative metallography is particularly suited for their examination, since the relative amounts of the two phases are very sensitive to their compositions. The method, however, is useless below about 350°C because of the inadequate resolution of the two constituents. Below 400°, however, the X-ray diffraction method is applicable, although it is of somewhat lower sensitivity in this system. The changes of composition that occur during quenching from above about 500°C entirely vitiate X-ray measurements at room temperature though they do not affect metallographic area measurements. The two methods overlap and supplement each other admirably. Both methods depend on the attainment of equilibrium composition of the two phases in a more or less intimate mixture and thus avoid the difficult problems of nucleation and long range diffusion involved in the conventional metallographic bracketing method. The alloys were melted from a master alloy made from re-electrolyzed cathode copper and Horsehead 99.99 pct Zn. Melting was done under a cover of either borax or charcoal and the alloys cast into a 7/8 in. sq graphite mold for the a-ß alloys or a 3/8 in. diam cylindrical graphite mold for the ß-? alloys. The a-ß alloys were rolled at 750°C to 5/8 in. sq; annealed for 24 hr at 800°C and quenched; then rolled and swaged at 200°C to 3/8 in. diam rods, annealed 24 hr at 200°C, quenched and cold rolled 2 pct reduction. This treatment was intended to obtain a small grain size and to produce many nuclei of the minor phase for growth on subsequent heat treatment. The unworkable ß-? alloys were given preliminary treatment by sealing in Vycor tubes in vacuum and annealing for 4 hr at 800°C followed by cooling in air. Samples of homogenized alloys were checked spectrographically for impurities, but the principal components were determined on samples subsequent to heat treatment. The impurities analyzed averaged approximately as follows: Ag, 0.0002 pct; Fe, 0.004; Si, 0.0008; Cd, 0.005; Mg, 0.0002; and Pb, 0.002. For metallography, samples of appropriate composition were cut into rods 5/8 in. long, sealed in pyrex tubes in vacuum and annealed for eight weeks at temperatures of 470°C and below, two weeks at 480°, 500°, and 600°C, and 4 hr at 700°C, followed by quenching in cold water. Temperatures were accurate to ±2°C. The cylinders were then machined to 8.7 mm diam and a slice weighing 1.5 g cut with a thin saw transversely from the center of each. This

Jan 1, 1953