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By Michael Tenebaum, C. C. Brown

In recent years, the importance of slag control in basic open-hearth operations has been universally recognized. To effect such control during the working period of the heat, methods have been developed to measure or estimate slag oxidation and slag basicity. While satisfactory rapid chemical methods have been developed to determine slag oxidation, no completely adequate method of evaluating basicity has yet been provided. The most generally accepted control methods of measuring slag basicity are based on visual cstimates. While considerable benefit may be derived from such estimates, the need for some measurable indication of slag basicity has become increasingly apparent. In a recent paper, Philbrook and Jolly suggested a promising technique for making the basicity determination. Their method consists of measuring the pH of a mixture of powdered open-hearth slag and distilled water. It was found that a relation could be established between the slag basicity and the alkalinity of the water mixture as measured by the hydrogen-ion concentration. The general procedure followed in making the measurements and the considerations involved in constructing the original curves are given in the paper of Philbrook and Jolly and need not be repeated. It is the purpose of this paper to discuss some of the factors considered in applying the pH measurements to actual slag control and to present some of the results of its apphcation. Factors Involved in Measuring pH of Water-slag Mixtures To facilitate the application of the pH control system, it was desirable that no alteration be made in the routine methods of sampling and crushing the furnace slag. Some of the factors considered before establishing a curve to relate slag basicity with the pH reading arc reviewed individually in the following paragraphs. Effect of Cooling Rate Under actual operating conditions there can be considerable variation in the temperature of the piece of slag crushed for the pH determination. To determine whether variations in crushing temperature or in cooling rate would affect the pH reading, a series of four samples was prepared from each of two separate slags. These samples represented conditions far more extreme than would actually be encountered. To obtain these samples, a thick pancake of slag was poured. One piece of this pancake was crushed immediately after it had solidified. Another piece was water-quenched and then crushed. A third piece was allowed to air-cool to room temperature before crushing. The fourth sample was prepared from a chilled slag. This sample was poured onto a heavy inclined steel plate at the

Jan 1, 1945

By A. J. Opinsky, J. L. Orehotsky, L. L. Seigle

TUNGSTEN incandescent lamp filaments possess a typical structure of elongated crystals generated upon heating the silica-alumina doped wire rapidly to 2200°C or above.&apos; It is known that these very long grains exhibit a preferred orientation, but there is disagreement in the literature about the direction. Rosi,2 and later Rieck; reported that the <135> direction of the large grains in doped wire tends to be parallel to the wire axis, but other investigators have reported that <110> is the preferred direction. Some further investigation of the orientations of large grains in tungsten wire is reported in the following. In the first series of experiments, 6-in. lengths of wire were heated rapidly in a bell jar. Current was passed through the wires and within 15 sec the wires had reached the grain coarsening temperature. 2 min was the annealing time. Wires were heated in hydrogen, nitrogen, and vacuum. Later, wires were heated in an evacuated tube furnace in which the tube was brought from 1000°C to the operating temperature within 25 sec and held 5 min at temperature. Temperatures were measured with an optical pyrometer. After heating, the wires were electro polished and etched, and the orientations of the large grains determined by the Laue back-reflection technique. Most of the experiments were carried out on a single spool of 5-mil silica-alumina doped wire, but a few tests were made with 5-mil thoriated tungsten wire and 10-mil undoped wire. 5-mil silica-alumina doped wires were reduced to smaller diameters by electropolishing for one series of experiments. Orientations of the large grains in silica-alumina doped wire heated in various atmospheres are presented in Figs. 1 and 2 as plots of the direction of the wire axis relative to the cube axes of the crystals. For most of the conditions studied, the preferred orientation cannot be described as a single direction, but the points might be said to group themselves about the arc passing through <110> and <113>. This arc is the trace of the (211) planes and contains the <135> and <124 as well as <011> directions previously observed by other investigators. The preferred orientation of large crystals in silica-alumina doped tungsten wire might be most generally described, therefore, by stating that a (211 ) tends to be parallel to the wire axis. This is true also for wires reduced in diameter by etching and furnace heated, Fig. 2, i.e., the recrystallization texture is apparently unchanged upon removal of the outer layers and substantially independent of the temperature gradient within the wire.

Jan 1, 1962

By A. K. Jena, M. O. Bever

The thermodynamic behavior of dilute solutions of copper, silver, and gold in liquid tin is not explained by current solution theories.1-3 The relative partial gram-atomic enthalpies, or heats of solution, of silver, gold, and platinum in liquid lead at 623°K have been measured in the investigation reported here. Their interpretation requires a modification of the regular-solution theory although lead-rich solutions may be expected to be simpler than tin-rich solutions. The liquid metal solution calorimeter used has been described.4 At the start of a run the bath consisted of 621 g of reagent-grade lead. Several calibrating additions of lead were made during a run; a value of 3.48 kcal per g-atom5 was taken for H623°K - H273°K Two runs were made with each of the solutes silver, gold, and platinum. Annealed wire samples of 99.999+ pct purity were used. Four to six samples each weighing 0.5 to 1,0 g were added from 273°K to the bath at 623°K and the associated heat effects were measured. The samples dissolved in approximately 3 min. No serious experimental difficulties were encountered. The heat effects of the additions in a run plotted against the average atom fraction of solute before and after each addition314 were linear functions of the concentration in lead of silver, gold, and platinum, respectively. By subtracting the difference between the heat contents of a solute element at 623° and. 273°K5 from the measuredheat effects, the partial gram-atomic enthalpy relative to the solid solute was obtained. The relativ: partial gram-atomic enthalpy at infinite dilution and the concentration dependence of the partial gram-atomic enthalpies obtained from the plots of vs atomic fraction x are listed in Table I. The relative partial gram-atomic enthalpy at infinite dilution of silver in lead of 5.46 kcal per g-atom at 623°K compares with values at 723°K of 5.74&apos; and 5.765 kcal per g-atom. These data yield a temperature coefficient of 3.0 cal per g-atom-OK. The partial gram-atomic enthalpy at infinite dilution of gold in lead at 623°K is 0.89 kcal per g-atom compared with 0.85 kcal per g-atoms (obtained by extrapolation) and 0.95 kcal per g-atom.5 By combining these values for 623°K with those for several other temperatures5" the temperature coefficient of was found to be 3.2 cal per g-atom-OK. No thermodynamic data are

Jan 1, 1968

By Charles S. Barrett, F. W. Steadman

Deformation bands of surprising regularity are found in large-grained poly-crystalline copper after cold-rolling (Fig. I). Individual bands frequently are large enough to permit a determination of their orientation by means of etch pits and an optical goniometer. Measurements have been made on 21 areas in seven different grains, and these, combined with X-ray studies of nine single crystals that had been cold-rolled after mounting in a polycrystal-line block, have contributed to a better understanding of the preferred orientations in rolled copper just as similar studies have for rolled iron1 and brass.2,3 Particular attention was given to determining orientations that are stable during rolling and to the manner of fragmentation and rotation of unstable grains. The possible role of twinning was also carefully investigated. The texture of polycrystalline copper after cold-rolling is well established by the pole figures that have been plotted by Schmid and Staffelbach,4 Iweronowa and Schdanow,6 and Brick and Williamson,8 all of which are in substantial agreement. There has been some divergence in the list of individual "ideal" orientations that have been used to describe the texture by these observers and others," although the orientation (110) [II2]—that is, (110) parallel to the rolling plane and [TIP] parallel to the rolling direction—is generally recognized as the most prominent orientation and (112) [III] one of the lesser orientations. Other orientations have been given by some observers as (236) [535], (100) [00I], and (110) [00I]. The texture of copper has also been described as (I35) [533].6,7 The sum of these orientations provides a reasonable approximation to the complete pole figure, but it does not follow that these specific orientations are necessarily of fundamental significance, for the choice of indices is arbitrary, within limits. Furthermore, a detailed investigation of the ideal orientations in cold-rolled iron discloses continuous ranges of equally favored positions rather than definite positions of high stability,&apos; and similarly Brick&apos;s observations in a single crystal of a brass2 suggest that all orientations in the range between (110) [II3] and (110) [II7] are about equally stable. Materials and Methods The material used was vacuum-cast electrolytic copper kindly supplied by L. L. Wyman, of the General Electric Co.* Slicec 1/2 in. thick and 21/2 in. square, cut from the ingot, were rolled with 50 per cent reduction per pass to final thicknesses between 0.02 and 0.04 in., and etched to develop cube-face etch pits suitable for goniometric work.8 The etch was light on some strips and deep in others.

Jan 1, 1942

By Benjamin Lustman, Robert F. Mehl

THE study of the high-temperature oxidation of pure metals, intensively pursued experimentally since the pioneer work of Pilling and Bedworth1 and supplemented by the recent theoretical work of Wagner2 is now well advanced. The important field of low-temperature oxidation-i.e., oxidation extending only through the temper color range of thicknesses with the formation of thin oxide layers in the range from o to 1000-2000 Angstroms-has not, however, reached so satisfactory a state, owing largely to the experimental difficulties that attend the formation and study of thin films; most of the work has been performed on abraded specimens whose surface irregularities approximated the thickness of the films formed. It has been pointed out that the rates of oxidation of different crystal faces are different and that the difference may be related to the orientation relationships that obtain between the metal crystal and the superimposed oxide crystal; it has also been suggested that this orientation dependence should manifest itself in rates of oxidation and perhaps also of corrosion in aggregates bearing preferred orientations. 3,4 An attempt to measure the rates of oxidation of different crystal faces of alpha iron demonstrated this difference in rate,4 but the dependence of rate on orientation was not simple; the method of measuring thickness, consisting of a color comparison with barium stearate multi-films of known thickness, was not wholly satisfactory. For these reasons it was felt that a study of the rate of oxidation of single crystals prepared with surfaces as smooth as possible, using a sensitive method giving true film thickness, should be profitable. Copper was chosen because of the ease of reduction of the primary oxide film and because the orientation relationships between metal and oxide and the composition of the oxide films formed at low temperatures are known; for thin films formed at low temperatures, Cu2O alone occurs.22-24 EXPERIMENTAL PROCEDURE Various methods of surface preparation were attempted in order to obtain a surface that would oxidize uniformly and reproducibly. Electrolytic polishing by the method of Jacquet5 and electrolytic and mechanical polishing followed by annealing in vacuum and in purified hydrogen at various temperatures were tested. The procedure finally adopted consisted in a fine metallographic polish followed by an anneal in purified hydrogen at temperatures of 900º to 1000°C. for 12 hr. or more. The surface so produced was very bright and smooth, with no trace of specular etching (though some grain-boundary etching was observed); indeed, fine scratches produced by the final polish were entirely removed by the high-temperature anneal.

Jan 1, 1941

By R. L. Huntington, Frank P. Vance, George F. Russell, Robert Thompson

With the advent of higher pressures in the operation of natural-gas transmission lines, the removal of water vapor from the gas has become increasingly important in order to prevent condensation or formation of gas hydrate from slowing down or stopping the flow of gas. Intelligent design of these dehydration or gas-drying plants has been hampered through the Iack of experimental data on the water vapor content of natural gas at elevated pressures. In view of this need, this present investigation was sponsored by the Southern Natural Gas Co. in the Chemical Engineering laboratories at the University of Oklahoma Research Institute. Experimental results were obtained on the water-vapor content of natural gas up to 2000 lb. per sq. in. at atmospheric temperatures. The water content at 2000 lb. is approximately two thirds as much as it is at 1000 Ib. Deviations from the ideal gas laws vary directly with pressure and indirectly with temperature. Introduction The removal of water vapor from natural gas is an important operation in connection with the production and transportation of this commodity because: I. Liquid water accelerates internal corrosion of a pipe line. 2. Accumulation of water at low points in a pipe line reduces markedly its capacity. 3. Gas hydrates, icy snowlike growths, form readily under high pressure in the presence of the lower hydrocarbons and water, often plugging up the pipe line. In order to design dehydration plants for stripping the gas of its water content, it is essential that the engineer. have a knowledge of the saturated or equilibrium water-vapor content of the gas to be processed. With the gradual increase of operating pressures around gas-producing wells and pipe lines, it was observed that the quantity of water recovered from dehydration plants or condensed in colder lines was considerably greater than had been expected from calculated contents, based on vapor-pressure data taken from steam tables. This observation prompted a number of investigators, for instance, Laulhere,3 Dea-ton,l and Hammerschmidt2 to carry out experimental work at pressures up to 600 lb. per sq. in. in order to determine quantitatively the water content of various gases. Sage, Lacey, et al.4,5 have recognized more recently the need for such data at higher pressures, but their work was done at temperatures of 100ºF, and higher. Since hydrate formation usually, if not entirely, occurs at temperatures below 100ºF., the present investigation was confined to the . lower temperature range at pressures from 600 to 2000 lb. per sq. in. gauge.

Jan 1, 1945

By Henry P. Ehrlinger, James C. Bradbury

Tripoli is a naturally occurring, very finely divided form of silica found chiefly in some midwestern and southeastern states and used commercially as fillers and abrasives. Definitions Tripoli is a microcrystalline, finely particulate, more or less friable form of silica that appears to be the product of leaching of siliceous limestone or calcareous chert. The term was originally applied to a deposit near Seneca, Mo., that resembled material of that name found near Tripoli in North Africa (Hovey, 1894). The two deposits were subsequently found to have different physical characteristics -the North African tripoli, now called tripolite, is a diatomite, composed of the siliceous skeletons of microscopic marine plants called diatoms, and the Missouri tripoli contains no diatom remains; the term tripoli, however, continued to be used for the Missouri material and is now applied in a general way to most silica deposits similar to it in characteristics and geologic origin. In commercial trade tripoli is commonly understood to designate material from the Missouri-Oklahoma field; silica from southern Illinois, the other major producing area, is referred to commercially as amorphous silica. Each term, however, may be used commercially for material, regardless of place of origin, that has the characteristics or uses commonly ascribed to the material from one or the other major producing area. For example, in the commodity price listings, Engineering and Mining Journal routinely lists under Tripoli, prices "f.0.b. Elco, III." and "f.0.b. Seneca, Mo., and Rogers, Ark.," and under Silica, amorphous, prices "f .o.b. Ill.," and "f .o.b. Dierks, Ark." Amorphous silica, the commercial designation given to southern Illinois tripoli, is, like the term tripoli, a misnomer. Mineralogically, the southern Illinois deposits are composed of microcrystalline quartz, and no amorphous material has been detected during X-ray and scanning electron microscope investigations (Leamnson, Thomas, and Ehrlinger, 1969; Thomas et al., 1970). Soft silica is another term that has been applied to Illinois and Tennessee tripoli, presumably to distinguish it from the more compact Missouri material. It has also been used in the ceramic trade to distinguish tripoli from "hard" silica, or silica flour, produced by pulverizing silica sand (Heinz, 1937). Rottenstone, produced commercially in Pennsylvania, is similar to tripoli in that a major constituent is finely particulate silica, and its uses are much the same as those of tripoli- as abrasives and fillers. The origin of rottenstone also is similar to that of tripoli-decomposition of a siliceous sedimentary rock. The parent rock is defined as a siliceous limestone (Gary, McAfee, and Wolf, 1972; Thrush, 1968) or as shale (personal communication). Heinz (1937) quotes a brief statement describ-

Jan 1, 1975

By S. A. Falconer

One of the outstanding achievements in connection with this country&apos;s war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too lowgrade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company&apos;s engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmen-ite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators—notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. Tungsten ORes Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of Course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1947

By S. A. Falconer

One of the outstanding achievements in connection with this country&apos;s war efforts has been the ability of our mining industry to supply from domestic sources many of the minerals of strategic importance that formerly were obtained principally from abroad. In order to meet the war-born demands for these scarce minerals, it has frequently been necessary to develop special methods for treating ores and waste products hitherto considered too lowgrade to be workable; and to improve the efficiency of older beneficiation processes. Important in this respect have been the recent technological advances in the field of froth flotation of nonsulphide minerals. Because of the refractory nature of many of these domestic ores, and, in many cases, the limited available technical data regarding their treatment, much research work has been necessary. The following examples describe the procedures and reagents used, and the results obtained, in certain laboratory flotation investigations conducted by American Cyanamid Company&apos;s engineers at the Cyanamid Ore Dressing Laboratory on ores containing such minerals as scheelite, manganese oxides and carbonate, ilmen-ite, brookite, kyanite, garnet, spodumene, mica, feldspar, celestite, fluorite, chromite, corundum, and cassiterite. In presenting these data, we wish to point out that many of the minerals listed have previously been tested, and their amenability to flotation reported, by other investigators—notably those of the United States Bureau of Mines. In some instances the procedures and reagents used in the treatment of some of the following described ores follow rather well-established lines, and with one or two exceptions, the reagents used were well known. However, many of the ores tested did not respond well to simple conventional procedures and it was necessary to adopt special methods of conditioning and desliming, reversal of the usual order of floatability of some of the minerals, multiple cleaning, etc., in order to secure separations. Except where otherwise noted, all numbered and trade-marked reagents mentioned in this paper are marketed by the American Cyanamid Co. or the American Cyanamid and Chemical Corporation. Tungsten ORes Tungsten minerals, vitally important in the war industries of the United States, rank high in the list of those we formerly had to import in order to supply our needs. Most of our domestic ores of tungsten contain scheelite as the valuable mineral. Today there are in the neighborhood of twelve tungsten operations in this country where flotation is used as the main or accessory form of benefication. It has, of Course, been known for some time that scheelite and other tungsten minerals respond to treatment by flotation.

Jan 1, 1947

By Norman Brown

It is suggested that the difference in ease of cross-slip among the fcc metals determines the relative amounts of [111] and [100] wire texture which occur in each metal. Since the ease of cross-slip is controlled by the stacking fault energy, it turns out that the amount of [111] texture should increase as the stacking fault energy increases. Arguments and existing data are presented to support the above suggestion. THE fcc metals generally have a dual texture, [11 and [loo], after wire drawing. As yet no fundament explanation exists concerning the variation of the amounts of each texture among the metals. Barrett&apos; has compiled data which show how the relative amounts of each texture vary from 100 pct [Ill] in the case of aluminum to 25 pct [l1] for silver. In this paper it is suggested that the value of stacking fault energy plays a major part in determining the amount of each type of texture. The double texture has its origin in the classical rotation of a single crystal under tension. An equilibrium position of the crystal is one in which three or more equivalent slip systems are operating simu taneously. Most crystals, initially, tend to rotate toward the [1ll] or the [l00] pole depending upon its initial orientation. This single-crystal behavior is essentially the same as the rotational behavior of the polycrystalline metal as worked out by Taylor.2 The next point to consider is whether the [Ill] or [100] orientation is more stable. There have been many discussions of this question3&apos;" which, in general, have lead to the conclusion that 11111 is most stable. For example, Pickus and Mathewson 4 suggested that a [Ill] texture produces more effective flow becake the [ 110] slip direction makes a smaller angle with the [111] than with the [loo]. A crude statistical argument will be presented which again favors the (1111 orientation. In order to maintain a pure [loo] wire texure, slip must occur in equal proportions in four of the six possible <110>slip directions. In order to maintain a pure [Ill] texture, slip must occur in equal proportions in only three of the six <110>directions. Since the <110> directions are the only slip directions in a fcc metal and if it is assumed that each of these six directions is equally probable, then the relative probability of a [1ll] texture vs a [l00] texture may be calculated. The statistical weight of a particular texture is the multiplicity of a texture times the probability of obtaining any one. The statistical weight for [Ill] is

Jan 1, 1962

By W. A. Griffith

The fundamental principles and modern techniques of experimental planning and data analysis, applicable to any type of research, are particularly important in flotation experimentation. Since they constitute the modern science of experimentation, they should be among the working tools of any scientist, research engineer, or plant operator engaged in flotation investigates. This chapter is a review of these principles and techniques. Equipment and procedures for the actual conduct of experiments will not be discussed here since these subjects are well covered elsewhere in this volume. Neither will any attempt be made to impart a working knowledge of statistical methods of data analysis since this would be impossible in the space allotted, and many excellent texts are available to the diligent inestigator.1-4 The objective here is simply to interest the reader in the application of statistical techniques to flotation experimentation by illustrating their utility in situations frequently encountered, and to point out the principles of experimental planning necessary for their proper use. Any conscientious metallurgist engaged in flotation experimentation or operations is well aware of the inherent complexity of the flotation process, and of the often frustrating difficulties this introduces into experimentation. The raw materials normally treated by the process are complex both physi- cally and chemically, and often highly variable even when from the same source. The flotation process itself is characterized by a very large number of potentially important process variables. Many of these are beyond the con- trol of the metallurgist, and some cannot even be measured quantitatively with available instruments. Those which can be measured and controlled with reasonable precision often produce effects which are intricately interrelated. Not only are the variables many, but the physical and chemical mechanisms by which they function are imperfectly under stood. To compound the difficulty, experimental techniques are relatively crude. Controls are not very precise, and the human factor looms large in most flotation experiments. These situations lead inevitably to experimental data of a relatively low degree of precision or reproducibility. Some are inclined to think that these conditions are unique to flotation experimentation. They are not. The experimental problems met by the agronomist, the biologist, the social scientist, and others are equally complex. Investigators in these fields pioneered in the development of methods for handling just such situations by proper experimental planning and the application of statistical methods in the analysis of data. Their pioneering work has grown into a well established modern science of experimentation which has spread into every field of science. This science is based upon statistical

Jan 1, 1962

By R. H. Fillnow, D. J. Mac

IT has been demonstrated that alloys in systems structurally analogous to steel undergo reactions during heat treatment similar to those of steel, and yet very little work has been done on such systems, particularly from the standpoint of isothermal transformation. The literature shows that most of the isothermal work has been done on copper-alu-minum alloys.&apos;-3 One paper has been reported on a eutectoid copper-silicon alloy,&apos; and one on iron-nitrogen alloys.&apos; There are no published reports of previous investigations on the isothermal transformation of a eutectoid beryllium bronze. At least two papers have been reported on isothermal age-hardening phenomena in beryllium-copper alloys of lower beryllium content.5,6 No information on eutectoid transformations in this alloy is given in Rimbach&apos;s book, "Beryllium." &apos; This paper reports the results of an investigation on the isothermal transformation characteristics of a eutectoid beryllium bronze. Materials Used and Procedure The eutectoid beryllium bronze used in this investigation was centrifugally cast at the Ampco Metal Co., Inc.. Milwaukee. Wis. A master beryl-lium-copier alloy, purchased from the Brush Beryllium Co., was used to make the beryllium addition to the copper. The alloy was melted under a protective carbon cover and Centrifugally cast into a graphite mold preheated to 920°F. Some trouble with segregation of beryllium in the melt was encountered but was eliminated by violent stirring during melting and pouring. Since very thin .specimens were used for the various heat treatments, only one casting of the four prepared was necessary for the complete isothermal study, thus eliminating any discrepancies caused by a change in composition. The analysis of this casting was 94.035 pct copper and 5.965 pct beryllium. A slight trace of iron was found. The castings were sawed into specimens approximately 3/32 in. in thickness. The specimens were first given an "austenitizing" heat treatment at 788°C, well within the single phase beta region, in a vertical tube furnace. The specimens were then quenched individually into an adjacent molten salt bath and held there for a definite time, after which they were quenched into water at room temperature. Temperature was held to ± 2°C in the salt bath. No homogenizing treatment was given the specimens other than the soak at 788°C. Despite the fact that this was a cast alloy, no evidence of segregation or coring was found in the microstructure of any specimen, either as cast or as heat-treated. Upon completion of the heat treatment, the speci-mens were subjected to metallographic examination

Jan 1, 1951

By E. A. Smith, E. R. Parker

METALLURGISTS and engineers have always been interested in the mechanism of high-speed deformation because metals are rapidly deformed in various applications and manufacturing processes. The deformation of metals by impact loads has recently engaged the attention of a number of investigators. Many of their results have not been disclosed but some of the published investigations1-8 have shown that the tensile strength, yield strength and elongation generally increase with increasing strain rate. The investigation reported herein is an attempt to determine the reason for this increase in strength and elongation. Single-crystal copper specimens were broken in tension at impact velocities up to 100 ft. per sec. The distribution of slip bands in the fractured crystals was found to depend upon the strain rate. In the bars broken at high speeds, the slip bands appear to be more numerous. This might account for the higher strength as well as the greater elongation. EXPERIMENTAL PROCEDURE Single crystals of copper (approximately 99.98 per cent) were made in graphite molds by the conventional method of lowering the mold out of the hot zone of a hydrogen furnace at a rate of one inch per hour. Solidification progressed from the bottom upward, forming a single crystal. The crystals were about 0.30 in. in diameter and 4 in. long. They were made into test bars by sliding threaded steel bushings over each end of a crystal and then flowing silver solder between the crystal and the bushing. The inside diameter of the bushings was slightly greater than the diameter of the crystals, to allow space for the silver solder. The bushings were placed so that the gauge length of the crystals was one inch. The assembly is shown in Fig. I, with two views of a fractured crystal. Annealed polycrystalline copper bars of similar shape were machined from solid stock. X-ray measurements were made on all single crystals to determine their orienta¬tions. The results are shown in Fig. 2, where the location of the axis of each specimen is indicated on a standard projection. The bars were broken in a commercial variable-velocity tension im¬pact machine, which has been described in detail elsewhere.7,8 The stress and strain were recorded by means of wire strain gauges and a special commercial oscillo-raph, also described in detail elsewhere.9,10 The equipment and method can be briefly described as follows. The impact machine consists of a motor-driven flywheel containing a two-pronged hammer. This hammer is held retracted in the flywheel

Jan 1, 1944

By C. R. McEwen

The displacement equations of Buckley and Lever-ett&apos; have been successfully applied to the prediction of oil recovery in frontal drives for a number of years. Commonly, the capillary pressure term is omitted from Leverett&apos;s fractional flow formula. The resulting satura-tion-vs-distance curves become multi-valued, however. Buckley and Leverett, recognizing that the neglect of capillarity was most likely the cause, proposed that this part of the solution he ignored. An ingenious method of propagating a discontinuity in place of the multi-valued portlon of the curve was devised by Cardwell using "non-capillary displacement theory". However, it would seem that a completc description of the displacement pracess would require the inclusion of capillary forces. Three publications on displacement theory have appeared in which capillary pressure was included. Ter-williger. et al&apos;, calculated saturation profiles which matched those which they observed when gas displaced water vertically downward. Based on their study, Jones-Parra and Calhoun5 roposed a method of computing saturation distributions sufficiently removed in time from the initial conditions so that all saturations in the flood front region were assumed to move with the same velocity. This latter assumption corresponds to the tangent construction on the flowing fraction-vs-satura-tion curve proposed by Welge." A numerical solution to the problem of water displacing oil from a water-wet porous medium was recently presented by Blair, ef at&apos;. The initial conditions included a uniform saturation slightly above interstitial water saturation. that is, the permeability to water ahead of the front was not zero. This appeared to result in a region of slowly rising water saturation ahead of the front, at least for the particular set of relative permeability and capillary pressure data used to illustrate the computation. The authors also postulated an "end-effect" at the outflow face of the system, whereby no water could pass out of the system until the water saturation had built up to a high value. The saturation profiles computed under these assumptions show water accumulating at the downstream end of the system while the flood front proper is still traveling toward the outlet. The purpose of this paper is to present the results of a numerical solution to the one-dimensional water-flooding equation in which no outlet end-effect is considered and where there is no flow of water ahead of the flood front. It should be noted that the contemporary paper of Fayers and Sheldon8 deals with the problem under discussion. For a thorough treatment including both capillarity and gravity the reader is referred to their paper.

By D. L. Martin, E. R. Parker

IN a previous paper, one of the authors observed that the rate of cooling from the anneal prior to testing greatly influenced the life of copper under sustained load at 200°C. Furnace-cooled bars of oxygen-free copper (with, and without silver) had a life four to twenty-five times that of the water-quenched specimens. The addition of 0.054 per cent silver to the oxygen-free copper increased the life at a stress of 20,000 lb. per sq. in. from about 2 hr. to 50 hr. Fractures in these bars were intercrystalline. An explanation was advanced to account for the profound influence of cooling rate on the rupture properties at 200°C. The suggestion offered was that at the high annealing temperature the minor constituents are distributed at random. By water quenching, this condition is maintained at room temperature, whereas furnace cooling permits some segregation at the grain boundaries. The higher concentration of the minor constituents in the grain boundaries results in a strengthening, so that a longer life at a given stress and temperature results. Small amounts of cadmium or manganese have also been found to increase the life of copper at 200°C., and to a much greater extent than silver .2 The increase in the long-time strength of copper resulting from small additions of cadmium or silver appears to be related, indirectly at least, to the higher softening temperatures of such alloys. The elements, such as silver or cadmium, which greatly increase the rupture life of copper also cause large increases in the softening temperature. As little as 0.05 per cent of cadmium or silver is sufficient to raise the softening temperature more than 100°.3,4 The effects of cooling rate and of minor constituents on the rupture properties are of considerable fundamental as well as practical interest; therefore a more detailed study of their nature was conducted and is reported in this paper. EXPERIMENTAL PROCEDURE Materials The materials studied in this investigation may conveniently be classified in two groups: one consisting of a wide variety of commercial coppers, and the other composed of special high-purity, laboratory-prepared coppers. The commercial materials were tested to determine whether or not the effect of cooling rate occurred with all coppers, whereas the high-purity coppers were investigated in order to establish a basis for evaluating the effect of minor constituents on the rupture properties. In Table I are given the analyses of the coppers tested. The samples I to 6 are commercial materials and were obtained for the most part from stock supplies.*

Jan 1, 1943

By D. E. Etter, J. E. Selle

The Pu-Ce phase diagram was determined by differential thermal analysis, metallography, and elechm-nricroprobe analysis. The dingram is chararterized by a eutectic with extensive solid solubility in the cubic Phases of both cerium and plutonium. No intermediate phases were found. Cerium is soluble in e plutonium to 16.0 at. pet Ce at 626OC nnd in d plcltoniurn to 23.0 at. pet at 613 "C, decreasing to 17.5 at. pet at room temperature. No solubility in the a, ß, or ? phases was jound, and the mininum cerium required to stabilize 5 plutonium to room temperature is 3.2 at. pet. The maximum solubility of plutonium in 6 cerium is 19.5 at. pet at 721OC, and the maximum soluhility of plutonium in ? cerium is 34.5 at. pet. Invariant points in the system are: a) eutectic at 626oC, L16.5 = E Pu16.0 + y Ce65.5; b) peritectoid at613oC, e Pu13.5 -y Ce65.5- d Pu23.0. AS part of a program aimed at the determination of the phase equilibria in the Pu-Ce-Cu ternary system, preliminary investigations were made of the three binary systems. A survey of the Pu-Ce binary system by differential therma1 analysis indi- cated several areas of disagreement with the published diagram,&apos; primarily in the shape of the liquidus surface. Consequently, a thorough investigation of the system was undertaken, and this report presents the results of the study. EXPERIMENTAL PROCEDURE Three methods of investigation were used: differential thermal analysis (DTA), metallography, and analysis with electron-microprobe X-ray analyzer (EMX). The EMX analysis was particularly useful for the determination of solvus lines. The DTA method was most useful for the determination of the liquidus curves. Metallography complemented both of these techniques. Materials. The cerium metal used for most of this work had a freezing point of 805°C. This material showed 15°C premelting, and was found metallographically to contain some unidentified in~lusions.2 The temperature of premelting is defined as the point at which the DTA curve breaks away from the base line, analogous to a curve obtained from a solid-solution alloy. Several compositions were prepared near the cerium end of the diagram with higher-purity material which had a freezing point of 800°C. etallographic analysis showed this material to be relatively free of inclusions and only 8°C premelting was observed. Major impurities were found by spectrographic

Jan 1, 1964

By R. I. Parsons, M. B. Standing, E. N. Lindblad

The recovery of the heavier components from a gas cap or retrograde pool is shown to be the greatest when the sand is cycled with a dry gas at a low pressure. This conclusion is in direct opposition to the belief that the most efficient production program is pressure maintenance and cycling at or near the dew point. The results are calculated from: (I) constant volume, variable composition pressure-volume-temperature tests on a mixture of trap gas and liquid from a producing well; (2) published equilibrium constant data and the measured composition of the dew-point material; and (3) the fact that in a sand section of homogeneous permeability, injected gas displaces reservoir gas nearly, quantitatively. The results are based on the simplifying assumption that variable permeability systems may be defined by the ratio of two statistical parameters, and that gas injected into an actual sand will behave as though the sand were composed of many layers, each of constant permeability. Introduction Pressure decline in gas-condensate type reservoirs is accompanied by the formation of a liquid phase throughout the reservoir. Over the past ten years the processing of the material from these types of reservoirs for the heavier hydrocarbon components and the return of the light fractions to the reservoir ("cycling") has become increasingly popular. It has often been stated that the purpose of such a program is to prevent the loss of the retrograde liquid phase formed in the reservoir. The purpose of this paper is to present the results of laboratory tests and computations concerned with several possible methods of producing a gas cap or condensate type of reservoir. The results show that the recovery of heavier hydrocarbons for this type of reservoir is not a maximum under conditions of cycling at or near the dew-point pressure. Instead, variations in permeability and the ability of the dry injected gas to revaporize condensate, point to cycling at a considerably reduced pressure as the optimum production-method. In addition the paper suggests a way of evaluating sands for their permeability variation. The calculations presented in the following sections of the paper are in terms of the production of the butanes and heavier fraction from the gas cap of a field which had an original pressure of approximately 3000 psi. Specifically, the calculations show: 1. To what extent the condensate formed in the reservoir after pressure decline can be recovered by the cycling of a dry absorber-plant gas through the sands. 2. Whether there would be greater recovery of hydrocarbons if cycling were instigated at the original reservoir pressure.

Jan 1, 1948

By Alexander Squire

A brief study of the effects of material and processing variations upon the tensile properties of steel formed from mixtures of iron and carbon was made in order to provide information regarding the properties obtainable in iron-carbon compacts as influenced by forming pressure, sintering temperature, and graphite particle size. Sintered steels formed from mixtures of iron and graphite have been studied by Stern,&apos; who investigated the effect of various percentages of graphite on compacts formed from electrolytic iron that were repressed and heat-treated after sintering. A further study, by Stern and Greenberg,l is concerned with the heat-treatment of steels formed by the car-burization of iron compacts, and Margolies3 has reported work on the simultaneous sintering and carburization of iron-powder parts. Glauch4 investigated the effect of various types of graphite on the properties of iron-carbon powder alloys but did not determine the effect of different particle sizes of the same graphite alloyed with different types of powder. In the investigation reported in this paper, powders typical of those produced by electrolytic deposition and the decar-burization of shotted steel scrap were used. The powders were mixed by tumbling in a jar mill with graphite powder ground to an average particle diameter of 2, 4, 6, and 16 microns (as determined by microscopic measurement). The properties of the iron and graphite powders are presented in tabular form as Table I. In order to obtain the maximum information from a minimum number of test specimens, the study was divided into two sections with one set of specimens treated identically in each section as a basis for comparison. In the first section, iron powder produced by the shotting and subsequent decarburization of scrap steel was mixed with 2-micron graphite powder, pressed at 50,000, 100,-000, and 200,000 psi, and sintered in hydrogen at 1200°C for the periods of time ranging from 15 to 120 minutes. In the second section of the investigation, electrolytic iron powder was mixed with graphite of an average particle diameter of 2, 4, 6, and 16 microns, pressed at 100,000 psi, and sintered at temperatures ranging from 1000° to r200°C&apos;. for periods of time of 30 to 180 minutes. By following this procedure an indication of the effect of the following variables upon the density and tensile properties of iron-carbon powder compacts was obtained: (I) forming pressure, (2) sintering time, (3) particle size of graphite powder, (4) sintering temperature, (4) type of iron powder.

Jan 1, 1947

By R. T. Hukki, A. M. Gaudin

Previous work on the principles of comminution has shown: (I) that the surface produced is proportional to work input (Rittinger law,1a-3); (2) that there is regularity to the weight distribution of the fragments according to size.4-10 In this paper it is brought out that the surface on the fragments is distributed in definite and simple relation to size. The experimental work has involved: I. Construction of an apparatus capable of measuring the surface of mineral fragments independently of the chemical composition of the fragments and independently of the site of the surface; 2. Refining the methods available for measurement of particle size; 3. Designing and building a crusher capable of operating on very small quantities of mineral, if necessary on single crystals, and in such fashion as to minimize handling losses of material. Complete experiments have been carried out with massive quartz and individual quartz crystals. partial experiments, lacking surface measurements, have been made with glass spheres, galena, sphalerite, fluo-rite, salt and coal. Introduction The existence of regularity in weight distribution with size was noted many years ago, especially by A. 0. Gates;&apos; the subject was also studied in detail by one of us.6 In the latter paper it was shown that rocks can be divided into two classes: homogeneous rocks, which show no preferential breaking, and heterogeneous rocks, which show preferential breaking at the grain size of the rock. It was shown, furthermore, that the fragments obtained by rupturing a homogeneous rock occur (in the fine range) in such abundance as to permit the writing of a relatively simple equation to relate the weight retained on a screen to the screen opening. With screens of which the openings are in constant ratio, the weight retained, w, is related to the screen size x by the equation w = Cxm [I] In this equation C and m are experimental constants. A plot of weight retained against particle size is a straight line of slope m if the scales for x and w are both logarithmic. In the fine range, the slopes of the size-distribution graphs plotted according to the method described above vary within a limited range. An inspection of a number of size-distribution data by various experimenters indicates that the slope very seldom exceeds 1.0, but is usually greater than 0.7. More recently, schuhmann8 proposed a method of charting that has so many advantages of its own that it has been used primarily in this work. For fine particles Schuhmann has found that the data are represented by the equation (x)m k [2]

Jan 1, 1947

By R. A., D. L. Sponseller, Flinn

Using specially del&apos;eloped titanium nitride crucibles and a pressurized syslem, it has been possible to determine the solzibilitv of liquid calcium in liquid iron and iron-base alloys. At 2925°F the solubility is 0.032 wt pet Ca in pure iron. The solubility is increased by aluminum, carbon, nickel, and silicon additions, and lowered by additions of gold. An inflection in the calcium-solubility curve occurs as carbon is added to iron. At approximately 0.87 Wt pet Ca the CaC, phase replaces liquid calcium, and the calcium concentration de- creases as more carbon is added to the iron. The maximum solubility, 0.36 wt pet Ca, was obtained in iron containing 10.5 wt pet Si. The data have important implications regarding the use of calcium in process metallurgy, as well as providing an interesting test of theories of metallic solutions. Reasonably good agreement is found with theories of Alcock and Richardson and of Wagner, and criteria are suggested which permit these theories to be applied more readily to systems of this type. AT the present time relatively little is known about the factors influencing solubility in liquid metals. Information of this type is important for such matters as the control of impurity levels in liquid metals, the use of magnesium in ductile-iron production, and the use of liquid-metal alloys as fuels and coolants in nuclear power plants. One important example of restricted solubility concerns the extent to which liquid calcium will dissolve in liquid iron. This is a matter of considerable interest in view of the strong potential of calcium for removing certain impurities in steel,. as well as the ability of calcium to desulfurize, inoculate, and produce spheroidal graphite in cast irons.&apos; Since ferrous materials normally contain other elements in addition to iron, the interactions of third elements with the Fe-Ca system are of interest. In view of the foregoing, this investigation was conducted to determine the solubility of liquid calcium in liquid iron and the effects of various third elements upon the solubility. For reasons of theoretical and engineering importance, the elements investigated were aluminum, carbon, gold, nickel, and silicon. Numerous attempts were made in the early part of the present century to determine the solubility of calcium in both liquid iron and steel, employing a variety of open-melt and closed bomb-type systems.2-4 From the results of these tests Wever concluded that calcium is insoluble in liquid and solid iron.5 These investigations were unsatisfactory in that they failed to insure the presence of a liquid layer

Jan 1, 1964