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By Bruce W. Gonser, Robert I. Jaffee

Recent work by the authors1 established the constitutional diagram of the gold-germanium system. Of particular interest in the simple euctectiferous system was the eutectic alloy at 12 per cent Ge, which melted at the very low temperature of 356°C and had an unusually fine eutectic structure. It was of interest to investigate the effect of third components on the melting point, microstructure, and strength of this alloy, and in this work the effect of copper is discussed rather completely, with less complete data on the effects of silver, platinum, nickel, and zinc. No reference in the literature has been found on ternary systems with gold-germanium. Materials and Alloying -4s in the work on the binary system, gold-germanium, the germanium used in this investigation was the cyanide-reduced, 99.9 per cent product, produced by the Eagle-Picher Co. Fine gold sheet from Handy and Harmon, pure platinum sheet from the American Platinum Works, copper magnet wire from Anaconda, nickel wire assaying 99.6 per cent Ni. and electrolytic zinc were used for alloying. To make the alloys, charges of the pure metals were put in a graphite crucible and melted in an atmosphere of pure hydrogen. The temperature was brought up to about I050 C, and the metal allowed to freeze in the crucible. Except with alloys containing zinc, melting losses were consistently less than a few milligrams. When zinc was a component, weight losses up to half the weight of the zinc present were incurred, and the alloy compositions were calculated by assuming the entire weight loss to be that of zinc. In all other cases the composition of the alloys could safely be taken as that of the charge. The ingots, as solidified, were segregated, the heavier primary phases being at the bottom and sides of the ingots and the lighter primary phases at the top, but by sectioning the entire ingot vertically for microscopic examination, this factor could be evaluated. Ingots for microscopic examination weighed one gram, and those for thermal analysis weighed three grams. Thermal Analysis In this work, the eutectic line composition and thermal arrests were desired, and, after microscopic exploration had established the position of the eutectic line at a given percentage of the third component, a thermal analysis was run at that composition. The method of thermal analysis used in the work on the binary Au-Ge system,' a method particularly well suited for a small quantity of material, was used in this work. Clearly defined arrests were obtained, although with some alloys containing platinum

Jan 1, 1946

By Robert I. Jaffee, Bruce W. Gonser

Recent work by the authors1 established the constitutional diagram of the gold-germanium system. Of particular interest in the simple euctectiferous system was the eutectic alloy at 12 per cent Ge, which melted at the very low temperature of 356°C and had an unusually fine eutectic structure. It was of interest to investigate the effect of third components on the melting point, microstructure, and strength of this alloy, and in this work the effect of copper is discussed rather completely, with less complete data on the effects of silver, platinum, nickel, and zinc. No reference in the literature has been found on ternary systems with gold-germanium. Materials and Alloying -4s in the work on the binary system, gold-germanium, the germanium used in this investigation was the cyanide-reduced, 99.9 per cent product, produced by the Eagle-Picher Co. Fine gold sheet from Handy and Harmon, pure platinum sheet from the American Platinum Works, copper magnet wire from Anaconda, nickel wire assaying 99.6 per cent Ni. and electrolytic zinc were used for alloying. To make the alloys, charges of the pure metals were put in a graphite crucible and melted in an atmosphere of pure hydrogen. The temperature was brought up to about I050 C, and the metal allowed to freeze in the crucible. Except with alloys containing zinc, melting losses were consistently less than a few milligrams. When zinc was a component, weight losses up to half the weight of the zinc present were incurred, and the alloy compositions were calculated by assuming the entire weight loss to be that of zinc. In all other cases the composition of the alloys could safely be taken as that of the charge. The ingots, as solidified, were segregated, the heavier primary phases being at the bottom and sides of the ingots and the lighter primary phases at the top, but by sectioning the entire ingot vertically for microscopic examination, this factor could be evaluated. Ingots for microscopic examination weighed one gram, and those for thermal analysis weighed three grams. Thermal Analysis In this work, the eutectic line composition and thermal arrests were desired, and, after microscopic exploration had established the position of the eutectic line at a given percentage of the third component, a thermal analysis was run at that composition. The method of thermal analysis used in the work on the binary Au-Ge system,' a method particularly well suited for a small quantity of material, was used in this work. Clearly defined arrests were obtained, although with some alloys containing platinum

Jan 1, 1946

By O. N. Cole, R. E. Davis, T. D. Brotherton

Pvfoperties of rubidium and cesium are compared with those of other alkali metals. Methods for the preparation of rubidium and cesium metal are reviewed briefly, ad hazards and safety precautions required in handling rubidium and cesium metal are described. SimPle methods for handling laboratory quantities of elemental rubidium ad cesium under oil and under argon are illustrated. CESIUM and rubidium were both discovered by Bunsen and Kirchoff in the years 1860 and 1861. Cesium was discovered while Bunsen and Kirchoff were making a spectrographic study of spring water from Durkheim, Germany. It was the first element discovered by this technique. The element was given the Latin name "caesius" for sky blue because of the color it imparted to flames. Elemental cesium was first prepared by Setterberg in 1881 through electrolysis of a molten mixture of cesium and barium cyanides.' In 1861, Bunsen and Mirchoff discovered rubidium while making a spectrographic study of the alkali content of lepidolite ore from Saxony. Two prominent dark red lines appeared in the spectrum and so the element was named "rubidius" or dark red. In 1861 Bunsen and Kirchoff first prepared elemental rubidium through the electrolysis of molten rubidium chl~ride.~ The alkali metals are very similar in their chemical and physical properties. They are the most active metals, and all exhibit a single oxidation state of one. They are so reactive that they are never found in nature in the elemental state. The reactivity of he metals increases with atomic number. Rubidiurn and cesium ignite spontaneously in air and react explosively with water. This extreme reactivity makes necessary special equipment and techniques for the safe preparation and use of the metals. The cation: of Group IA can be separated from the metallic cations of other groups with relative ease, but the separation of the individual alkali cations is much more difficult because of their close chemical similarity. This close chemical and physical similarity of alkali metals can be inferred from the atomic radii, oxidation numbers, and ioni-zation potentials shown in Table I. A difficult but the most practical physical method of separating the elemental alkali metals from one another is by distillation. Only lithium has a boiling point sufficiently far-removed from the boiling points of the other alkali metals to make this method of separation feasible without elaborate and expensive equipment. This method is not used, however, for lithium because it possesses sufficient chemical dissimilarity from the other alkalies for it to be separated relatively easily as lithium hydroxide monohydrate or as lithium carbonate. Francium, the last member of the group, has no known stable isotopes. The naturally occurring

Jan 1, 1962

By John T. Eash

During the course of the war the supply of tin in this country has steadily decreased and a continued effort has been made since the beginning of the emergency to use alloys that are either tin free or contain appreciably lower quantities of it. Even with the use of emergency materials, the tin supply has become particularly acute, and it is estimated that after recovery of the far eastern mines probably one to two years will be required before our normal annual supply is attained. One of the major tin-consuming fields is the bronze industry. Recommendations were made several years ago by the War Production Board toward the use of bronzes of lower tin content and manganese bronze and yellow brass for the customarily used tin-bronze alloys. The substitution of 88-5-5-2 copper-nickel-tin-zinc for composition G received considerable attention before the war, and consequently this alloy and modifications of it have been adopted for some current structural and pressure castings requiring high mechanical properties. Another of the commonly used bronzes is the 10 per cent tin 10 per cent lead copper alloy for heavy-duty bearings. It has been known for some time that about 2.5 per cent nickel could be substituted for an equal amount of tin with retention of equivalent casting and tensile properties; however, it was desirable that a still greater conservation of tin be made. Consequently the present paper deals with the development of an alloy of low tin content that could be used for bearings. Selection or Composition While the final criterion of the suitability of an alloy for a bearing must of course be determined by practical applications where all the ramifications of service conditions are encountered, certain short cuts in the initial selection of compositions are necessary to avoid an extensive and time-consuming investigation. The present program has been to match certain metallurgical properties of the 80-10-10 bronze that have been shown by previous investigations to be related to good bearing qualities. Such properties as microstruc-ture, hardness, compressive yield strength, ductility, and castability have been considered, and certain simple wear tests have been made. Of the readily assessed characteristics desired in a good bearing alloy, one can be certain that a uniform distribution of lead is required in a leaded bronze. It has generally been found that segregation of lead is one of the chief difficulties with this type of material. Tin has a powerful effect on lead distribution, and with 10 per cent present produces a random distribution of chunky particles, such as are shown in Fig' 1. I' In the tin bronze contains the hard alpha + delta

Jan 1, 1946

By John T. Eash

During the course of the war the supply of tin in this country has steadily decreased and a continued effort has been made since the beginning of the emergency to use alloys that are either tin free or contain appreciably lower quantities of it. Even with the use of emergency materials, the tin supply has become particularly acute, and it is estimated that after recovery of the far eastern mines probably one to two years will be required before our normal annual supply is attained. One of the major tin-consuming fields is the bronze industry. Recommendations were made several years ago by the War Production Board toward the use of bronzes of lower tin content and manganese bronze and yellow brass for the customarily used tin-bronze alloys. The substitution of 88-5-5-2 copper-nickel-tin-zinc for composition G received considerable attention before the war, and consequently this alloy and modifications of it have been adopted for some current structural and pressure castings requiring high mechanical properties. Another of the commonly used bronzes is the 10 per cent tin 10 per cent lead copper alloy for heavy-duty bearings. It has been known for some time that about 2.5 per cent nickel could be substituted for an equal amount of tin with retention of equivalent casting and tensile properties; however, it was desirable that a still greater conservation of tin be made. Consequently the present paper deals with the development of an alloy of low tin content that could be used for bearings. Selection or Composition While the final criterion of the suitability of an alloy for a bearing must of course be determined by practical applications where all the ramifications of service conditions are encountered, certain short cuts in the initial selection of compositions are necessary to avoid an extensive and time-consuming investigation. The present program has been to match certain metallurgical properties of the 80-10-10 bronze that have been shown by previous investigations to be related to good bearing qualities. Such properties as microstruc-ture, hardness, compressive yield strength, ductility, and castability have been considered, and certain simple wear tests have been made. Of the readily assessed characteristics desired in a good bearing alloy, one can be certain that a uniform distribution of lead is required in a leaded bronze. It has generally been found that segregation of lead is one of the chief difficulties with this type of material. Tin has a powerful effect on lead distribution, and with 10 per cent present produces a random distribution of chunky particles, such as are shown in Fig' 1. I' In the tin bronze contains the hard alpha + delta

Jan 1, 1946

By Ottokar Hofmann

In tank-lixiviation, the extraction of the silver from chloridized ore by solutions of hyposulphite salts is performed by filtration. The ore-particles are kept stationary, while the solvent moves down through the mass of ore. The quickness of extraction, other conditions alike, is in direct proportion to the rapidity of the movement of the solvent through the ore. The solution, if left in contact with the ore without moving, displays but very little solving energy. If the filtration is interrupted for ten or twelve hours, and thus solution and ore are left in complete contact for that length of time, it mill be found that, when filtration is started again, the outflowing solution is but very little more saturated with silver than it was at the time of interruption, and that the ten or twelve hours were almost a perfect loss in the total time of extraction. Notwithstanding the long contact, the solution had not become saturated with silver chloride to its full solving capacity. A rapid movement of the solvent through the ore is essential to a quick extraction. This fact is well known ; and the endeavor of leachers has been to hasten extraction by increasing the rate of filtration. Siphons, vacuumpumps and other devices have been used with more or less success; but none of them have given full satisfaction. I have found that, if chloridized ore is brought into rapid contact with a proper volume of moving sodium hyposulphite solution, the silver chloride contained in the ore dissolves almost instantly, and that it is rather the volume of the solvent than its concentrated state which produces this effect. Such favorable conditions cannot be attained in tanks. The rapidity with which a certain volume of the solvent can be brought into contact with the ore-particles is limited by the speed with which the solution descends through the ore; and thus the leaching-time in tanks cannot be shortened beyond the limit set by the filteringcapacity of the ore. In a trough, however, these favorable conditions can be attained by gradually introducing the ore into the moving stream of the solvent. The ore can thus be brought into

Jan 1, 1888

By Raymond D. Sloan

Dropping from third position among the oil-producing states of the nation in 1942, Oklahoma ranked fourth in 1943 with a total output of 121,431,ooo bbl., a decline of 11.9 per cent from the previous year's total of 137,792,000 bbl. Production ranged from a maximum of 346,900 bbl. daily in February to a low of 322,800 bbl. daily in October, and at the close of the year was averaging 330,000 bbl. daily from 52,096 wells, or an average of 6.3 bbl. per well. The state's well, average at the close of 1942 amounted to 6.7 bbl. At the turn of the year, it appeared reasonable to assume that Oklahoma's producing rate would continue its downward trend during 1944 unless reversed by greater than normal discoveries. To Jan. I, 1944, Oklahoma has produced 5,188,466,-ooo bbl. of crude oil. Development and Exploration A total of 1287 wells was drilled in 1943, representing an increase of 77 wells, or 6.4 per cent over the preceding year's total of 1210. Of the wells completed, 587 (45.6 per cent) were oil wells with an average initial production of 319 bbl.; 127 (9.9 per cent) were gas wells with an average initial of 8,639,000 cu. ft.; and 573 (44.5 per cent) were dry. A total of 333 wildcats was drilled (25.9 per cent of all wells), an increase of 13 (4.1 per cent) over the 1942 total of 320. Of the*wildcats drilled, 46 (13.8 per cent) were oil wells with an average initial production of 235 bbl.; 27 (8.1 per cent) were gas wells with an average initial of 8,249,-ooo cu. ft.; and 260 (78.1 per cent) were recorded as failures. Reconditioning of wells throughout the state led to a total recompletion of 230 wells. Of these, 131 were oil wells with a combined initial production of 8360 bbl., 31 were gas wells with a total initial of 211,950,000 cu. ft., and 68 were abandoned. The 46 successful wildcats opened 33 new producing areas, one of which produced from three separate horizons, and led to the development of production in new horizons in 11 old pools. While none of the 1943 discoveries have as yet developed into what might be termed major pools, the West Moore pool, in Cleveland County, and the West Edmond pool, in Oklahoma County, are the two outstanding new areas opened to production. The West Moore pool, sec. 29, 10 N., 3 W., discovered in December 1943, was completed for an initial production of 248 bbl. of oil in 3 hr. through small tubing chokes in the second Wilcox sand from 8787 to 8800 ft. One well was drilling in this area at the close of the year. The West Edmond pool, an April discovery in sec. 32, 14 N 4 W., is producing from the Hunton lime at a depth of approximately 6950 ft., the world's deepest Hunton lime pool. To the end of the year, 15 oil wells had been completed, with no gas wells and no failures. Accumulated production to Jan. I, 1944, amounted to 474,300 bbl. of 41" gravity oil. There were 29 active operations in the field at the end of the year. The West Edmond and West Moore pool discoveries established the first commercial production west of the Granite Ridge,

Jan 1, 1944

By Raymond D. Sloan

Dropping from third position among the oil-producing states of the nation in 1942, Oklahoma ranked fourth in 1943 with a total output of 121,431,ooo bbl., a decline of 11.9 per cent from the previous year's total of 137,792,000 bbl. Production ranged from a maximum of 346,900 bbl. daily in February to a low of 322,800 bbl. daily in October, and at the close of the year was averaging 330,000 bbl. daily from 52,096 wells, or an average of 6.3 bbl. per well. The state's well, average at the close of 1942 amounted to 6.7 bbl. At the turn of the year, it appeared reasonable to assume that Oklahoma's producing rate would continue its downward trend during 1944 unless reversed by greater than normal discoveries. To Jan. I, 1944, Oklahoma has produced 5,188,466,-ooo bbl. of crude oil. Development and Exploration A total of 1287 wells was drilled in 1943, representing an increase of 77 wells, or 6.4 per cent over the preceding year's total of 1210. Of the wells completed, 587 (45.6 per cent) were oil wells with an average initial production of 319 bbl.; 127 (9.9 per cent) were gas wells with an average initial of 8,639,000 cu. ft.; and 573 (44.5 per cent) were dry. A total of 333 wildcats was drilled (25.9 per cent of all wells), an increase of 13 (4.1 per cent) over the 1942 total of 320. Of the*wildcats drilled, 46 (13.8 per cent) were oil wells with an average initial production of 235 bbl.; 27 (8.1 per cent) were gas wells with an average initial of 8,249,-ooo cu. ft.; and 260 (78.1 per cent) were recorded as failures. Reconditioning of wells throughout the state led to a total recompletion of 230 wells. Of these, 131 were oil wells with a combined initial production of 8360 bbl., 31 were gas wells with a total initial of 211,950,000 cu. ft., and 68 were abandoned. The 46 successful wildcats opened 33 new producing areas, one of which produced from three separate horizons, and led to the development of production in new horizons in 11 old pools. While none of the 1943 discoveries have as yet developed into what might be termed major pools, the West Moore pool, in Cleveland County, and the West Edmond pool, in Oklahoma County, are the two outstanding new areas opened to production. The West Moore pool, sec. 29, 10 N., 3 W., discovered in December 1943, was completed for an initial production of 248 bbl. of oil in 3 hr. through small tubing chokes in the second Wilcox sand from 8787 to 8800 ft. One well was drilling in this area at the close of the year. The West Edmond pool, an April discovery in sec. 32, 14 N 4 W., is producing from the Hunton lime at a depth of approximately 6950 ft., the world's deepest Hunton lime pool. To the end of the year, 15 oil wells had been completed, with no gas wells and no failures. Accumulated production to Jan. I, 1944, amounted to 474,300 bbl. of 41" gravity oil. There were 29 active operations in the field at the end of the year. The West Edmond and West Moore pool discoveries established the first commercial production west of the Granite Ridge,

Jan 1, 1944

By Richard H. Olson

"Rarely in our technological society does the discovery of a new class of inorganic materials result in such a wide scientific interest and kaleidoscopic development of applications as has happened with the zeolite molecular sieves." That opening sentence in a landmark volume on zeolite molecular sieves by D. W. Breck (1974), is, if anything, an understatement. Zeolites were recognized as a new group of minerals in the 1750s, but it was not until 1930 that the first analysis of the crystal structure of a zeolite mineral was made. In the late 1940s research workers at Union Carbide Corp. began a program of zeolite synthesis and study which has resulted in one of the major research achievements of all time. Naturally, with the vast research and development efforts devoted to the synthetic molecular sieves, Union Carbide became concerned in the mid-1950s about its position should minable deposits of natural analogues be discovered. Zeolite minerals have diverse origins, and even a brief discussion of these is beyond the scope of this paper. The early work on zeolites was confined to igneous rock occurrences (e.g., amygdules and veins) which were formed by "space-filling;" these crystals tend to be euhedral, thereby rendering them appealing to both mineralogists and collectors. During the first year or so of Union Carbide's exploration (which began in mid-1957) attention was devoted solely to such igneous, occurrences. A landmark paper by Bramlette and Posnjak (1933) heralded the potential significance of the occurrence of zeolite minerals as alteration products of vitric ash and similar materials. In the summer of 1958, full attention was directed by Union Carbide to the search for deposits of this type in the western United States. Since then, such exploration has been continuous by both commercial firms and private parties. The future economic potential for natural zeolite deposits seems to be restricted to those of the "open-and-closed system" types as described by Sheppard (this chapter). Therefore, this and the following discussions will concentrate upon these types; the other types of zeolites in sedimentary rocks (e.g., deep-sea sediments, burial metamorphic, and hydrothermal) will be, for the most part, ignored. Despite the relative cheapness of natural zeolite deposits as compared with the cost of synthetic molecular sieves, there has been minimal development of zeolite mining in the US over the past 25 years or so. Mumpton (this chapter) discusses the present commercial utilization of natural zeolites and their future potential in detail, but perhaps the following will serve as useful background. In the early days of synthetic molecular sieve research and production, the efforts were concentrated largely upon such high-value applications as physical separation of components in a stream (based upon molecular size and geometry) and in catalysis. Due to a number of reasons (some of which are difficult for an outsider to understand), natural zeolite ores (beneficiated or not) have not made substantial inroads upon the use of the higher-priced synthetic molecular sieves for the foregoing applications, but this is not to say that such a condition will exist forever. Furthermore, in view of the many other uses which are now known, or which loom in the future, the competitive position of the natural zeolites vs. the more expensive

Jan 1, 1983

By J. H. Swisher

In measuvements of the solubility of nitrogen in fer-rilic Fe-P alloys, tile nitrogen solubility is found to be Less in pIrospliorus-bearing alloys than in pure iron. The reduction in solubility is about 20 pct in a 1.0 wt pct P alloy at 1300°C and about 30 pct in a 0.23 wt pct P alloy at 440°C. Diffusion coefficient measurements at 1150 and 585°C show that phosphorus also decreases the nitrogen diffusivity in iron. In previous work on the Fe-P-N system, phosphorus was found to reduce the nitrogen solubility in liquid iron slightly.&apos; Indirect evidence for similar behavior in a Fe at low temperature was obtained by Dickenscheid and Brauner.&apos; These authors found that phosphorus reduces the height of the internal-friction peak due to dissolved nitrogen. The results of Dickenscheid and Brauner were confirmed by J. C. Swartz of this Laboratory in a single internal-friction experiment using the same specimen stock as in the solubility measurements described below. In the present investigation, the solubility of nitrogen in a fer rite-stabilized Fe-1.0 wt pct P alloy was measured in the temperature range from 800" to 1300°C. Additional experiments were performed in the temperature range from 440° to 585°C, using an Fe-0.23 wt pct P alloy and NH3-H2 gas mixtures. EXPERIMENTAL The experiments were performed in a vertical tube furnace wound with platinum wire. For experimental temperatures of 800°C and above, a mixture of 5 pct Hz in N2 was used as the reacting gas. The gas mixture was prepurified from oxygen by passage over platinized asbestos at 450°C, and subsequently over anhydrone to remove water. Flow rates of the gases were measured with capillary flow meters. The temperature was measured before and after each experiment with a Pt/Pt-10 pct Rh thermocouple. The specimens used for the high-temperature solubility measurements were in the form of rectangular plates, 0.534 by 1.6 by 3.8 cm. The specimens were cleaned in trichloroethylene and annealed for 2 hr in hydrogen at the beginning of each experiment. In measuring the nitrogen solubility, the specimens were held in the reacting gas until equilibrated, then cooled in a water-cooled copper block at the bottom of the furnace. The time needed for equilibration at 1150°C was determined by measuring the average nitrogen content of the 1.0 pct P alloy as a function of reaction time. As will be described, the nitrogen diffusivity in the alloy at 1150°C is only slightly less than its calculated diffusivity in pure iron. At temperatures other than 1150°C, the reaction time used in measuring the nitrogen solubility was about twice the calculated equilibration time for pure iron at the same temperature. With a few exceptions, the procedure for the low-temperature solubility measurements was the same as that described above. The compositions of the NH3-H2 gas mixtures were determined by collecting gas samples from the gas train and analyzing them for NH3 by titration with HC1. The specimen thicknesses were less than those used for the high-temperature experiments, eg., 0.124 and 0.051 cm for measurements at 585° and 440°C, respectively. Nitrogen concentrations were obtained by chemical analysis, using the Kjeldahl method. The Fe-P alloys were made by adding ferrophos-phorus to electrolytic Plastiron (Type 104 A). Commercial ferrophosphorus, containing 3 pct Mn and 0.35 pct Si as the major impurities, was first purified by melting under an FeO slag. In a separate heat, the electrolytic iron was melted and vacuum-carbon-deoxidized prior to making the ferrophosphorus addition. The principal impurities and their concentrations in weight percent in the 1.0 pct P alloy are as follows: Mn, 0.01; Si, <0.01; C, 0.01; 0, 0.003; and N, 0.0012. The impurity levels in the 0.23 pct P alloy are con-

Jan 1, 1968

By D. S. Eppelsheimer, D. N. Williams

The cold rolled textures of iodide titanium and of three samples of commercial titanium were examined using the Schulz-Decker Geiger counter technique. The iodide titanium and two of the three samples of commercial titanium showed a (0001) [1010] texture rotated 30&apos; toward the transverse direction about an axis in the rolling direction. The third sample of commercial titanium showed a double texture. THE metals of the hexagonal system tend to deform similarly if the c/a ratios are similar. Thus titanium, zirconium, and beryllium, with c/a ratios of 1.601, 1.590, and 1.570, respectively,l should have similar cold rolled textures. The cold rolled texture of high purity iodide titanium has been described as (0001) [1010] rotated 30" toward the transverse direction about an axis in the rolling direction.&apos; The texture of zirconium has also been reported as (0001) [1010] with a transverse rotation from the ideal position of approximately 30" about an axis in the rolling direction." This texture differs from that reported for titanium however since a continuous spread of (0001) poles toward the transverse direction was reported rather than distinct (0001) maxima 30" from the rolling plane normal. Beryllium has a texture similar to that of zirconium although the angle of transverse rotation of the (0001) poles is much less.&apos; These three metals thus show a common type of cold rolled texture, as yet unexplained, which can be described as (0001) [1010] with various degrees of rotation toward the transverse direction about an axis in the rolling direction. Since titanium showed the greatest degree of rotation from the (0001) [1010] position, the cold rolled texture of titanium was re-examined using a semiquantitative Geiger counter X-ray technique to obtain more accurate experimental data from which a theoretical interpretation of this new type of hex- agonal rolling texture could be developed. The cold rolled textures of iodide titanium and of three samples of commercial titanium were determined. Table 1 gives the analyses of the titanium samples. Experimental Procedure Preparation of Samples: Prior to the final rolling operation each of the samples was given an initial reduction of approximately 50 pct and annealed to remove the gross effects of any previous treatments. Samples were annealed in vacuum, high purity helium, and air to determine whether annealing atmosphere had any effect on the cold rolled textures developed. All samples were annealed 1 hr at 800°C. Grain size determinations were made using the formula, 1.075 in which n is the number of grains counted in an area A (in sq mm) and M is the magnification of the area counted.&apos; This formula gives the diameter between opposite flats assuming hexagonal grains. At least three areas containing more than sixty grains each were counted in each grain size determination. Rockwell B hardness readings were made on the annealed samples. The results of the measurements of

Jan 1, 1954

By John Wulff, David A. Stevenson

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

Jan 1, 1962

By Arthur Gray

THE thermal analysis of a metal or alloy is ordinarily made with the aid of heating and cooling curves, in which transitions are indicated by the rapid changes in curvature that accompany .changes in the rate of heat absorption or evolution. Analysis by the method that depends on the change in thermal expansivity is not customary, partly, at least, because of the difficulties involved in making the necessary measurements. However, under certain circumstances, the dilatometric method of analysis may possess advantages over the thermometric method that will justify the additional trouble required. The addition of 1 per cent. of zinc to an alloy has been found to produce, upon the volume changes that take place during transition, effects that suggest the possibility of using the dilatometric method of thermal analysis as a rather sensitive means of obtaining chemical information. Although the illustrations presented in this paper are drawn from data obtained during an investigation of dental amalgams, similar phenomena can doubtless be observed with other alloys. Some of the results found during an investigation made in 19171 have been confirmed by data on the thermal expansivity of amalgams published by Souder and Peters of the Bureau of Standards in reporting tests of dental materials.2 Although the Bureau of. Standards made experiments for the purpose of discovering effects of including zinc as one of the constituents of a dental alloy-a matter much discussed in dental literature but without the presentation of reliable experimental evidence to support the views of ;either side-the reports of the test made by the Bureau give the impression that certain striking phenomena associated with the presence of zinc were not noticed. Among such phenomena are those connected with the conditions that determine whether or not a specimen of amalgam becomes covered with droplets from which crystals develop.

Jan 9, 1920

By D. F. Kelsall

The hydraulic cyclone, in simple or modified form, is finding increasing application in metallurgical processing. In this article, the author considers several aspects of conventional applications, less conventional applications and some potential uses of modified cyclones. Information concerning the mechanism of separation within a cyclone and the effect of the major variables is summarized. During the past twenty years, and especially in the last decade, hydraulic cyclones have found increasing application in metallurgical processing as classifiers and, under special circumstances, as thickeners. To a more limited extent cyclones have been used to extend heavy, or dense, medium separation into the finer size ranges, and several attempts have been made to separate dispersions of immiscible liquids with a view to use in the field of liquid-liquid extraction. A large proportion of published work reports incomplete data, applicable only to particular systems. The more useful papers, covering data of relatively wide significance, have been reviewed recently in considerable detail1,2 and no attempt will be made to cover the same material in the present paper. However, before considering several aspects of conventional application, less conventional applications and some potential uses of modified cyclones, it is considered pertinent to summarize information relating to the mechanism of separation within a cyclone and the effect of the major variables. LIQUID FLOW PATTERNS At any point within a simple cyclone the liquid velocity may be resolved into three components, i.e., the tangential or swirling velocity (v), the vertical velocity (w), and the radial velocity (u). The relative values of these components at selected positions within a typical cyclone have been established for water. 3 The extent to which similar flow patterns exist in systems of considerably higher viscosity, or apparent viscosity, operating under conditions of reasonable pressure drop, is not known with precision, but indirect evidence indicates that up to approximately five centipoise there is no marked change. Beneath the bottom of the vortex finder, envelopes of constant tangential velocity are cylinders coaxial with the cyclone, and, at any horizontal level, starting from near the conical wall, this component of velocity increases with decrease in radius (r) according to the relationship vrn = constant (where 0 < n < 1) This holds to regions near the center of the cyclone where v reaches a maximum value at a radius somewhat smaller than that of the inside wall of the vortex finder. At this point, the centrifugal acceleration, v2/r reaches a maximum value. As the radius is further decreased the tangential velocity decreases so that v = r. Above the bottom of the vortex finder there is a tendency for the first relationship to persist to near the outside wall of the vortex finder, until v reaches a maximum and then decreases rapidly as the wall is approached. The two most significant features of the vertical velocity distribution are an approximately conical Table I. List of Symbols v = liquid tangential velocity at any point in the cyclone w = liquid vertical velocity at any point in the cyclone u = liquid radial velocity at any point in the cyclone r = radius from cyclone axis to any point ? = half angle of conical portion of the cyclone ?= fluid viscosity d = particle diameter s = liquid specific gravity p = particle specific gravity d50 = the particle diameter which distributes 5090 to overflow, 50% to underflow e = overflow diameter, in. b = feed diameter, in. G = gpm of feed slurry

Jan 1, 1963

By Milton H. Fies

THE writer wishes to acknowledge at the outset his great sense of obligation to those who contributed so broadly and expertly to the preparation of this paper: Dr. Albert DeSmaele, Chairman of the Board of Directors of Socogaz, Belgium; Dr. Julien Venter, Director of the National Institute of Coal Mining, and Coal Utilization Industry, Belgium; Dr. Roger Loison, Chief Engineer, French National Coal Research Board, France; and Dr. Erich Sarapuu of the Sinclair Coal Co., Kansas City, Missouri. Liberal use has been made in this paper of a recent publication on Russian, Italian, Belgian, and French experiments prepared jointly by the Centre d&apos;Etudes et Recherches des Charbonnages de France (Cerchar) and the Institut National de I&apos;Industrie Charbonnière of Belgium (Inichar) .l The writer is particularly indebted to Dr. E. T. Wilkins, of the Fuel Research Station, London, and to Mr. James L. Elder, of the Alabama Under- ground Gasification Experiment at Gorgas, Alabama, for their unfailing patience and effective support. Not only did these experienced and capable men edit and revise this discussion, but much of its content is a direct contribution quoted in full from their memoranda. Without the assistance of all these colleagues, this presentation would not have been possible. It has been a privilege to serve and work with them and to acknowledge repeatedly their loyal cooperation. The recovery of the energy inherent in coal beds throughout the world has been done through the years by methods that today may be justly regarded as primitive. While the techniques of coal mining through the application of machines and the enhancement of information and skills have advanced to an extraordinary extent, particularly during the past 20 years, the underlying means is essentially the same as when man first began to mine coal. Despite this progress in the manner of coal mining, it continues today as a hazardous, toilsome, grimy task. Coal mining per se has advanced at a greater and more rapid stride in the past 25 years than the mining of any other mineral, but the basic method is fundamentally the same as it was the first day a miner took a pick into his hands many centuries ago. This situation presents a challenge to mining engineers everywhere, from

Jan 1, 1953

By Brij M. Moudgil

Disposal of fine coal refuse is one of the major technical problems which could adversely affect growth and development of the coal industry. At present one of the most: common methods for disposal of fine coal refuse slurry involves impounding the slurry behind dams. However meeting new federal and state government regulations for building, maintaining and reclaiming these impoundments in addition to terrain and space considerations render this technique to be only marginally competitive with other disposal methods. The coal industry has been actively engaged in developing alternate disposal techniques which are economically feasible and environmentally acceptable. A review of coal refuse disposal problem and current refuse disposal practice both in the eastern and western coal fields is presented. Various promising techniques being developed for economical and safe disposal of fine coal refuse slurry are also discussed.

Jan 1, 1980

By W. S. McCain, B. A. Wilcox, A. H. Clauer

The creep and creep-fracture behavior of a Ni-200-2Th0, alloy has been studied over the temperature range 816° to 1038°C and stress range 4000 to 19,000 psi Specimens having their axes either parallel or transverse to the final sheet-rolling direction were tested in air, and the apparent activation energy for creep was found to be 92 kcal per mole, regardless of specinien orientation. The stress dependence 01- the steady-state creep rate, was satisfied by where n depended on orientation; n = 9.7 for rrzaterial transverse to the rolling direction and n = 24.3 for material parallel to the rolling direction. In the latter case, the relation was also valid. The rupture strength of material parallel to the rolling direction was -1.5 times gveater than the transverse rupture strength. Several tests in vacuum revealed that here the creep rate was higher and rupture life lower than for comparable tests in air. THERE is an increased interest today in producing improved dispersion-hardened alloys for high-temperature structural applications. This had led various materials designers to modify existing alloys, such as thoriated nickel. One system that has received considerable attention is based on chromium additions to Ni-ThO2, with the obvious motive of improving the oxidation resistance. Another effect of chromium is that of lowering the stacking-fault energy, y, of nickel. For example, the addition of 30 wt pct Cr decreases y from -225 erg per sq cm for pure nickel1 to -70 erg per sq cm.&apos; This decrease in y could have several effects on the deformation behavior. There is some evidence that cross slip of dislocations around Tho2 particles is a mechanism of tensile3 and creep4 deformation in TD Nickel (Ni + 2 vol pct ThO2) at temperatures below 0.5 the absolute melting point of nickel, T,. A decrease in ? by chromium additions should increase the difficulty of cross slip. Also it has been suggested that the high-temperature (T > 0.5Tm) rate-controlling creep process in "recrystallized" Ni-Tho2 alloys is the climb of edge dislocations over Tho2 particles.5 According to weertman6 a decrease in the stacking-fault energy should decrease the dislocation climb velocity resulting in a decreased steady-state creep rate. Thus, chromium additions to recrystallized Ni-Tho2 alloys would be expected to decrease the creep rate, all other conditions being constant. However, a difficulty arises when the stacking-fault concept is applied to high-temperature creep of dispersion-strengthened metals which are produced on a commercial or semicommercial scale. This occurs because the materials are processed so that they have a high-stored energy of cold work, and the other substructural effects could obscure any influence of stacking-fault energy per se. An example of an alloy with a high stored energy of cold work is TD Nickel bar. This material has a fibrous grain structure (1 I diam by 10 to 15 p long), and the structure is stabilized by the ThO2 particles. Annealing at high temperatures, e.g., 3 hr at 1300°C, causes no recrystallization or grain growth.4 Previous work by the authors4 showed that the high -temperature creep behavior of TD Nickel could not be related to any simple dislocation theory of creep, and this probably was associated with the complex initial structure of the material.

Jan 1, 1968

By R. H. Maes, R. E. de Strycker, J. J. Jacobs

A simple method, based upow density measurements, has been perfected in order to determine the critical temperature of liquid miscibility gaps. Applied to the Pb-Cu system, it yielded a value of 980"C for the critical tempevature of the miscibility gap in this system. In the Pb-Cu-As system, the immiscibility between lead and coppev evolves towards a miscibility gap be-tween lead and copper arsenides; the liquation temperatures were determined joy different avsenic contents and values up to 1065°C were found. Combining these results with those given by the clzemical analysis of liquid samples taken at dqj.event temperatures, it has been possible to make a cowzplete determination of the liquid miscibility gap in this ternary system. In the Pb-Cu-Fe-As system, a ternary miscibility gap has been discovered; for some compositions, the molten and slowly cooled alloys separated into three layers: an Fe-As alloy, a Cu-As alloy, and a lead-rich layer. ThE Pb-Cu-Fe-As system is of interest for the study of the behavior of speiss or arsenical alloys in the lead blast furnace. The speisses produced in lead metallurgy generally have complex compositions, but they may be considered, in a simplified way, as a mixture of copper, iron, nickel, and cobalt arsenides; there is often an excess of metallic constituants, and lead is also present. Speisses liquate from lead at various temperatures according to their composition; according to industrial experience, iron speisses are already distinctly separated from lead bullion at temperatures of the order of 1100°C, whereas copper speisses only begin to liquate from lead at much lower temperatures, near their solidification points, which were never accurately determined until now. Besides these considerations of practical interest, the present study is of importance for the knowledge of liquid miscibility gaps. Particularly the data of the literature about critical temperatures of liquation are incomplete and present sometimes considerable disparities; a method has been perfected in the present work to determine these temperatures with accuracy. MISCIBILITY GAP OF THE LEAD-COPPER SYSTEM Review of Literature. The generally admitted outline of the Pb-Cu equilibrium diagram is shown by Fig. 1. This figure, with its numerical indications, is taken from the review of Hansen and ~nderko;&apos; compositions are given in weight percent, as will be the case in the remainder of this paper. Between 36 and 87 pct Pb, Pb-Cu alloys separate into two layers, in the liquid state. The critical temperature of liquation has been much disputed in earlier studies, where values up to 1500°C were claimed; but a reliable study of ~ohnen,&apos; based upon differential thermal analysis, gave a value of 990°C; this rather low value was verified by a recent study of Schiirmann and Kaune? based upon thermodynamical properties of the Pb-Cu alloys, which predicted a value of 1002°C. Liquid miscibility gaps were also studied by means of chemical analyses. Satisfactory results were generally obtained with the method consisting in taking samples of the two liquid layers in equilibrium and submitting them to chemical analysis; however, this method becomes delicate near the critical temperature. With this technique, Friedrich and waehlerts ob-

Jan 1, 1968

By John J. Secretary Egan

The present list of problems relating to the physical chemistry of steelmaking has been prepared by the Committee on the Physical Chemistry of Steelmaking, from answers to a questionnaire submitted to a number of metallurgists engaged in both industrial and educational work throughout the United States. The purpose of the project is to make available to research laboratories a list of problems, all reduced to their simplest terms, the solution of which would aid in creating a better understanding of the steelmaking process. It is not intended to restrict the problems to practical steelmaking. The list also includes the study of the properties, and their correlation, as well as the physical and chemical reactions, of all substances that occur or that may be in any way associated with steelmaking operations, such as metallic substances, refractories, nonmetallic inclusions, and the constituents of slags. Many of the problems can be carried out in university or other research laboratories. Others may be most successfully attacked by cooperation of the research men with the operating personnel. It is the Committee&apos;s earnest wish that this cooperation be fostered. It is requested that investigators who are working on any of the problems listed and who anticipate future publication of their results, notify the Secretary of the Committee that such investigation is in progress. Suggested additions to the present list are also requested. The Committee is undertaking to act as a clearing house for information regarding the topics in this field that are being actually studied. Interested persons are invited to correspond with the Secretary. I. Data involved in the state of equilibrium for the various systems (laboratory work, almost entirely). A. Specific heats, heats of formation, entropies and free energies of various PURE ELEMENTS OR COMPOUNDS; ALSO CERTAIN TYPICAL SLAGS AND REFRACTORIES I. Determination of specific heats and entropies of oxides, sulphides, nitrides, etc, over a wide temperature range. 2. Determination of free energies of oxides, sulphides, nitrides, etc., over a wide temperature range. 3. Determination of the heats of formation of the oxides, sulphides, nitrides, etc. 4. Determination of the thermodynamic properties of the more important mineral-ogical constituents of the basic open-hearth slags such as calcium silicates, calcium phosphates, calcium ferrites, manganese silicates, FeO and Fe2O3. 5. Determination of the specific heats of open-hearth slags, including liquid silicates, if possible.

Jan 1, 1941

By John J. Secretary Egan

The present list of problems relating to the physical chemistry of steelmaking has been prepared by the Committee on the Physical Chemistry of Steelmaking, from answers to a questionnaire submitted to a number of metallurgists engaged in both industrial and educational work throughout the United States. The purpose of the project is to make available to research laboratories a list of problems, all reduced to their simplest terms, the solution of which would aid in creating a better understanding of the steelmaking process. It is not intended to restrict the problems to practical steelmaking. The list also includes the study of the properties, and their correlation, as well as the physical and chemical reactions, of all substances that occur or that may be in any way associated with steelmaking operations, such as metallic substances, refractories, nonmetallic inclusions, and the constituents of slags. Many of the problems can be carried out in university or other research laboratories. Others may be most successfully attacked by cooperation of the research men with the operating personnel. It is the Committee&apos;s earnest wish that this cooperation be fostered. It is requested that investigators who are working on any of the problems listed and who anticipate future publication of their results, notify the Secretary of the Committee that such investigation is in progress. Suggested additions to the present list are also requested. The Committee is undertaking to act as a clearing house for information regarding the topics in this field that are being actually studied. Interested persons are invited to correspond with the Secretary. I. Data involved in the state of equilibrium for the various systems (laboratory work, almost entirely). A. Specific heats, heats of formation, entropies and free energies of various PURE ELEMENTS OR COMPOUNDS; ALSO CERTAIN TYPICAL SLAGS AND REFRACTORIES I. Determination of specific heats and entropies of oxides, sulphides, nitrides, etc, over a wide temperature range. 2. Determination of free energies of oxides, sulphides, nitrides, etc., over a wide temperature range. 3. Determination of the heats of formation of the oxides, sulphides, nitrides, etc. 4. Determination of the thermodynamic properties of the more important mineral-ogical constituents of the basic open-hearth slags such as calcium silicates, calcium phosphates, calcium ferrites, manganese silicates, FeO and Fe2O3. 5. Determination of the specific heats of open-hearth slags, including liquid silicates, if possible.

Jan 1, 1941