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By G. R. Fitterer

NonmEtallic inclusions in steel have received much attention by metallurgists during the past few years. Many investigators have been emphatic in stating their belief that these impurities are the chief causes of steel failures, while others think that their effects are negligible. One of the main reasons that definite information on the effects of these impurities is lacking is that no reliable method has been developed for the exact determination of the amounts of these different impurities in steel. Some valuable new information has been brought out by a reliable method for nonmetallic inclusions which has been developed at the Pittsburgh Experiment Station of the U. S. Bureau of Mines, in cooperation with the Carnegie Institute of Technology and the Metallurgical Advisory Board. This procedure satisfactorily extracts some of the more common inclusions from steels, thus enabling the investigator to correlate steel failures with inclusion content. Although the data given herein are the first to be published on the subject of the electrolytic extraction method, the interest in the subject is evidenced by the fact that it is already being used by some 20 to 30 steel companies for their various purposes. Some of the comments received from these laboratories indicate that the method is highly satisfactory: the unfavorable comments, when traced to their sources, have been found to be based on some small mistake made in either installation or operation. The chief discrepancy seems to have occurred in attempts to apply the method to the extraction of inclusions from alloy steels. The procedure can be used only for the plain carbon steels and for such low alloy steels as those containing the usual amount of copper (0.2 to 0.3 per cent). Steels containing the carbide-forming alloys such as chromium, tungsten, etc., present far too many difficulties for the accurate determination of inclusions. Luckily, the iron and manganese carbides do not offer any difficulties and no contamination of the oxide-sulfide residue results, It is highly probable that some modification of the following

Jan 1, 1931

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

By Robert L. Bates

On April 2 and 3, 1970, more than 100 geologists attended the Sixth Annual Forum on Geology of Industrial Minerals at Ann Arbor, Mich. After this brief appearance, the Forum apparently ceased to exist- but it didn't really, and another spring will see it again in action, in another corner of the country. The organization might be characterized as the country's largest permanent floating conference on the geology of industrial minerals. What is the Forum, where did it come from, and what is it up to? The idea originated in 1964 with a small group in the Department of Geology at Ohio State University, Columbus. This group felt that a forum was needed for the exchange of geologic information on industrial rocks and minerals. They envisioned an approach-which has subsequently been adhered to--that would be dominated neither by geological academics interested in theoretical problems nor by practical engineers concerned with processing large tonnages of rock. It was proposed to focus attention on the middle part of the spectrum, especially on practical problems of geological occurrence and how these problems affect extraction and use. In terms of the standard rock-products flow sheet, which starts with a truck unloading into the primary crusher beneath the words 'from quarry,' it was proposed to focus geological attention on what is beyond the primary crusher, out in the quarry.

Jan 1, 1970

By Frank G. Norris, William C. Marshall

The term "total operation" is meant to include problems that cannot be answered from the standpoint of either the blast furnace or the open hearth separately but must be studied by considering the interrelations of these two processes. There are other ways of expressing this idea, such as reference to the blast furnace and the open hearth as an integrated process or by emphasizing the interrelation and interaction of the two processes. Much progress has been made in metallurgy and other fields by breaking complicated processes and reactions into simpler parts and studying each of these intensively. This intensive study frequently is done under the controlled conditions of the laboratory experiment. The entire process is understood better by this specialized study of each of its parts. This procedure is so satisfactory that an understanding of unit operations is a fundamental requirement of chemical engineering. Much discussion of the open-hearth process is in terms of one heat or one furnace. By this is meant that the conclusions apply to one furnace, wherever it may be. Furnaces seldom occur singly; they are located in groups and these groups are located in steel plants having characteristic blast-furnace equipment. Problems that are affected by the number of furnaces operating, by the number of blast furnaces in the plant and by the fact that the open- hearth shop is dependent on the bla furnace capacity rather than on its o needs for the amount of iron available among those which, in contrast to "u operations," we have chosen to call "to operations." Many of these problems, such as cha ing delays and the general mechani problem of material handling, are familiar that merely to define " total op ations" brings them to mind. These pr lems are of such importance that alrea they have received careful thought 2 study and probably will merit furt study. As will be shown later, these mechan problems are so intimately related metallurgical problems of total operati that the effect of certain changes cannot ascribed with certainty to either a mech ical or a metallurgical cause entirely. Although the problems coming under general term of "railroading" are inclu in the problems of total operations, ' others are selected for the discussion of paper, One of these is strictly a problem composition; the other is strictly a prob of tonnage production. The problem of phosphorus is pres whenever basic open-hearth slag is used the blast-furnace burden. This practice not secured universal acceptance chi because of difference in preference for h manganese or low-manganese pig iron hjgh-manganese (2.00 per cent) iron is to made, open-hearth slag as a source manganese is usually cheaper than m

Jan 1, 1943

By William C. Marshall, Frank G. Norris

The term "total operation" is meant to include problems that cannot be answered from the standpoint of either the blast furnace or the open hearth separately but must be studied by considering the interrelations of these two processes. There are other ways of expressing this idea, such as reference to the blast furnace and the open hearth as an integrated process or by emphasizing the interrelation and interaction of the two processes. Much progress has been made in metallurgy and other fields by breaking complicated processes and reactions into simpler parts and studying each of these intensively. This intensive study frequently is done under the controlled conditions of the laboratory experiment. The entire process is understood better by this specialized study of each of its parts. This procedure is so satisfactory that an understanding of unit operations is a fundamental requirement of chemical engineering. Much discussion of the open-hearth process is in terms of one heat or one furnace. By this is meant that the conclusions apply to one furnace, wherever it may be. Furnaces seldom occur singly; they are located in groups and these groups are located in steel plants having characteristic blast-furnace equipment. Problems that are affected by the number of furnaces operating, by the number of blast furnaces in the plant and by the fact that the open- hearth shop is dependent on the bla furnace capacity rather than on its o needs for the amount of iron available among those which, in contrast to "u operations," we have chosen to call "to operations." Many of these problems, such as cha ing delays and the general mechani problem of material handling, are familiar that merely to define " total op ations" brings them to mind. These pr lems are of such importance that alrea they have received careful thought 2 study and probably will merit furt study. As will be shown later, these mechan problems are so intimately related metallurgical problems of total operati that the effect of certain changes cannot ascribed with certainty to either a mech ical or a metallurgical cause entirely. Although the problems coming under general term of "railroading" are inclu in the problems of total operations, ' others are selected for the discussion of paper, One of these is strictly a problem composition; the other is strictly a prob of tonnage production. The problem of phosphorus is pres whenever basic open-hearth slag is used the blast-furnace burden. This practice not secured universal acceptance chi because of difference in preference for h manganese or low-manganese pig iron hjgh-manganese (2.00 per cent) iron is to made, open-hearth slag as a source manganese is usually cheaper than m

Jan 1, 1943

By R. H. Kolb

A long term project at Shell Development Co.'s Exploration and Production Research Laboratory has been the improvement of the accuracy and the ease of BHP measurements. As a result of these efforts, two complete and separate systems have now been built for the automatic logging of BHP variations. The first of these is a small-diameter instrument suitable for running through production tubing on a single-conductor well cable. During the development of this instrument, as much emphasis was placed on providing a high degree of usable sensitivity and repeatable accuracy as on obtaining the advantages of surface recording. The second system combines the benefits of automatic, unattended recording with the convenience of a permanently installed Maihak BHP transmitter.' THE CABLE INSTRUMENT For many years the standard instrument for BHP determination has been the wireline-operated Amerada recording pressure gauge or one of several other similar devices. This gauge records on a small clock-driven chart carried within the instrument, and although relatively precise readings from the chart are possible, they are difficult to ob-tain. a Both the maximum recording time and the resolution of the time measurements are limited by chart size, and when a slow clock is required for long tests, the precision of the time measurement is often inadequate. Since it is impossible to determine the data being recorded until the gauge has been returned to the surface, wasted time often results when a test is protracted beyond the necessary time or when it is terminated too soon and must be re-run. Clock stoppage or other malfunctions which would be immediately apparent with surface recording remains undetected with down-hole recording; the test is continued for its full term with a consequent loss in production time. As new uses for subsurface pressure data evolved, the shortcomings of the wireline instrument became increasingly apparent, and the concurrent development of a surface-recording pressure gauge and the associated high-pressure well cable service unit' was undertaken. Description of the Instrument Because of its ready availability and advanced degree of development, the Amerada bourdon-tube element was chosen as the basic pressure-sensing device. This element converts a given pressure into a proportional angular displacement of its output shaft, and a suitable telemetering system was designed to measure accurately the extent of this displacement and to transmit the measurement to the surface and record it. The telemetering system furnishes a digital record printed on paper tape by an adding machine-type printer. The present arrangement provides a resolution of one part in 42,000 over the angular equivalent of full-scale deflection, giving a usable sensitivity of better than 0.0025 per cent of full scale. An additional refinement simultaneously records on the tape the time or the depth of the measurement, also in digital form. When the instrument is placed in operation, an adjustable programer can be set to initiate a read-out cycle automatically at selected time intervals. When subsurface pressures are changing rapidly, readings may be recorded as frequently as once every 10 seconds; when pressures are more nearly stabilized, the period between readings may be extended to as much as 30 minutes. Because the instrument is surface-powered as well as surface-recording, the maximum period of continuous logging is (for all prac. tical purposes) unlimited. The subsurface instrument is a tubular tool, 1 1/4-in. in diameter and 6.5 ft in length, operating on 12,000 ft of conventional 3/16-in. IHO logging cable. The transmitting section, mounted above the bourdon-tube element in place of the regular recording mechanism, contains no fragile vacuum tubes or temperature-sensitive transistors. This unit has been laboratory-tested to 1 0,000 psi and 300°F and has performed dependably during a number of field operations. The down-hole transmitting arrangement can be fitted to any standard Amerada pressure element, regardless of range and with no modification of the element itself. Calibration To obtain a repeatability commensurate with the sensitivity and resolution of the instrument, it was necessary to develop a special calibrating technique. The manufacturers of the Amerada recording pressure gauge claim an accuracy of only 0.25 per cent of full scale, which is a realistic figure for normal calibrating and operating procedures. An exhaustive investigation was made of the errors inherent in the bourdon-tube element, itself, independent

By JOHN S. HEARDING

ON the Minnesota Ranges, 600 million tons of material have been moved in the past three years to produce 172 million tons of direct-shipping iron ore. Increasing wage rates and cost of equipment and supplies, coupled with the larger amount of waste material to be moved in comparison with the quantity of ore make it imperative that tile industry adopt all practices and methods which will enable it to move earth at progressively lower costs. Drilling. Prior to and during the war practically all blastholes drilled were 6-in. in diameter and put down by drills using strings of tools weighing from 2000 to 3000 lb. Present trends indicate that heavier drilling equipment making 9-in. holes wit11 3000 to 6000 lb tools will be more economical. Holes up to 12 in. diameter will be made with this equipment. Forging and hardening practices for bits to increase footage is receiving attention. One manufacturer expects to market 9-in. bits having sintered carbide inserts in the reaming and cutting edges. Oxygen and oil to burn holes in the rock are being tested for making blastholes at a considerably greater speed than can be obtained with a blasthole drill on the same size hole. To dale, however, the cost has been prohibitive.

Jan 1, 1949

Jan 1, 1985

By Frederick O?Neil

SCOPE OF THIS REPORT THE object of this paper is to describe the present status and possibilities of liquid oxygen as an explosive based upon the investigations, research and practical work of the Ingersoll-Rand Co., and of the Air Reduction Co., from early in 1922 to date. The following work was done. 1. A study of the history and physical theory of L. 0. X. as an explosive. (No attempt will be made in this paper to give the history or theory, as this has already been covered by the literature on the subject.) 2. An investigation of the use and the practice with L. 0. X. in the iron mines of Lorraine where L. 0. X. has its largest application in Europe. Although L. 0. X. is extensively employed in the; iron mines of Lorraine, many of the mines using it exclusively, and blasting with it a total of approximately three million tons of iron ore per year, the fact that the mining practice in Lorraine1 is to drill comparatively shallow holes and blast only a few holes at a time, renders the data obtained there of very little value in estimating the possibility of replacing dynamite with L. 0. X. in American mining methods. In fact, in the iron mines in Lorraine, L. 0. X. replaced black powder, or its equivalent. 3. Laboratory research work on properties of absorbent materials. 4. Work in the Bureau of Mines explosive laboratory at Pittsburgh, Pa., on the properties of L. 0. X. cartridges. 5. Practical work underground with L. 0. X. cartridges in the Witherbee-Sherman iron mines at Mineville, N. Y. 6. Practical work in the quarries of the Calcite Quarry Co., Myers-town, Pa. 7. Practical blasting in several quarries and open-pit mines.

Jan 2, 1926

By Chas. Y. Clayton, Francis B. Foley, W. E. Remmers

DuRing the summer of 1919, the late Dr. Henry M. Howe, then Chairman of the Division of Engineering of the National Research Council, organized a committee to obtain a better insight into the behavior of carbon steels under the influence of various treatments by a proper control of the time and temperature factors. During part of 1919 and 1920, work in connection with this investigation was carried on at Dr. Howe's laboratory at Bedford Hills, N. Y. During 1921 there was an enforced hiatus in the work, occasioned by the illness which resulted in Dr. Howe's death in 1922. At that time one of the present authors compiled the results of the work which had been done and this was published in 1923.' Following the publication of this work, it seemed desirable to carry on in the same manner an investigation of steel of C 0.75 per cent., which steel had not been as fully treated as had the other steels of C 0.34 and 0.52 per cent., used in the published work. Furthermore, certain unusual results have been obtained in the treatment of C 0.52 per cent. steel by quenching and drawing, and repetition of this part of the work seemed advisable. This has been done during the past year at the School of Mines and Metallurgy of the University of Missouri at Rolla, Mo., by a cooperative undertaking of the School and the Bureau of Mines, working in conjunction with the Committee on Heat Treatment of Carbon Steels of the National Research Council. The present paper is a report of the results obtained in this work.

Jan 1, 1926

By R. P. Agarwala, M. S. Anand

Using residual activity technique, the diffusion of palladium, silver, cadmium, indium, and tin in alunzinum has been studied in the temperature range of 400" to 630°C. The diffusivities (in units of square centimeters per second) have been expressed as: IMPURITY diffusion in aluminum,1-9 silverand lead5 for cases of low solid solubility of the impurity in the host metal has yielded frequency factors in the range of l0-6 to l0-9 sq cm per sec whereas the activation energy is practically half the self-diffusion activation energy value. From the observed values of frequency factor, activation energy, and entropy of activation, it has been suggested' that these solutes are not diffusing by vacancy or interstitial mechanisms but by a mechanism which should be consistent with such low values of the diffusion parameters (Do and Q). However in spite of extensive work on these types of systems, the mechanism of diffusion is still not well understood. The present investigation on the diffusion of palladium, silver, cadmium, indium, and tin in aluminum has been carried out to throw further light on the diffusion mechanism in systems, where the solid solubility is very low (except for the case of silver). The results are discussed on the basis of solid solubility and the structural changes involved owing to the presence of the solutes in aluminum solid solution. An attempt has also been made to apply the existing theories of charge5-8 and size8 difference between the solute and the solvent. EXPERIMENTAL PROCEDURE Specimens (1/2 in. diam by 3/8 in. high) were machined out of pure aluminum (99.995 wt pct) rod obtained from Johnson Mattheys. They were sealed under vacuum in quartz tubes and annealed at 620° C for several hours; the grains thus developed were sufficiently large to eliminate the possibility of diffusion along the grain boundaries. The flat ends were prepared carefully after polishing as described previously,10 Radioactive nitrates of cadmium, indium, and tin and chloride of palladium containing, respectively, cd115, 1n114, sn113, and pd103 were dissolved in distilled water and mixed with 30 pct acetone. By means of a micropipet a drop of this solution was placed on a smoothly polished and lightly etched surface of the specimen. Due care was taken to see that the solution spread uniformly on the surface of specimen without trickling down its sides. Radioactive silver was elec-trodeposited using a AgCN-KCN bath. The amount of sample deposited in all the cases was not more than 0.1 µ thick. The samples were then sealed in quartz tubes in vacuum. The cadmium samples were sealed in a purified argon atmosphere to avoid evaporation. The samples were then diffusion-annealed. The temperature of annealing varied between 400° and 630°C and was controlled to ±5°C. On heating to -400°C,the deposits of cadmium, indium, and tin, which were of the order of 0.1 p in thickness, were converted to their respective oxides. The contribution of oxygen present in the lattice of aluminum due to these oxides has been calculated and found to be less than 10 ppm in all cases. Oxide method has already been used by other workers11'12 in diffusion studies without any controversy on the issue. However, in some of these investigations, metallic deposition was also tried. The diffusivities calculated from these measurements were found to agree very well with the diffusivities obtained by using the oxide method. Thus it is assumed that the measured diffusivities represent true diffusion coefficients. Since palladous chloride decomposes at about 500°C, the deposited samples which were to be diffusion-annealed below 500°C were heated in vacuum for a very short time at 500°C to allow the decomposition of palladous chloride to palladium metal. Time taken in decomposition of nitrates to oxides and chloride to metal was negligibly small as compared to the period of the diffusion anneals. The residual activity technique13 was used to study the diffusion profiles where thin layers from the specimen surface were removed by grinding it parallel to a flat surface on a 600-grade carborundum paper. The specimen was washed, dried, and weighed, the differ -ence of the weight being the measure of the thickness of the layer removed. After each such abrasion and weighing, the total residual activity on the surface of the specimens was measured by counting 0.656, 0.94,

Jan 1, 1968

By R. Maddin, A. Lawley

Single crystal Mo-Re alloys (99.99+ purity), grown by electron bombardment floating zone heating, were deformed in tension at temperatures from -196° to +200°C. At -196oC, Mo-6 pet Re and Mo-20 pct Re alloys deform by slip on systems of the type (101) [1ll]. Above-78oC, the operative slip system is of the type (112) [111], (101) [1ll], or (211) [1ll], depending upon orientation. Mo-39 pct Re alloys deform by twinning and slip at all test temperatures with a (112) [111] type twinning system. Critical resolved shear stress for slip and twinning is calculated as a function of composition and temperature, and the mechanical properties compared with those of less Pure polycrystalline alloys. HEXAGONAL close-packed rhenium, c/a = 1.615, is highly soluble in molybdenum. The bee molybdenum-rich solid solution extends to approximately 42 at. pet Re* at 2500°C,' Fig. 1. Recent work on polycrystalline alloys has shown conclusively that the addition of rhenium to molybdenum improves both the fabricability and the low-temperature ductility.2"5 Similar behavior is observed for W-Re and Cr-Re alloys.5 Initially, Geach and Hughes2 found that the Mo-30 pct Re alloy could be cold rolled to approximately 90 pct reduction before the onset of cracking. The remarkable effect of the rhenium was later confirmed by Jaffee et al. 3-5 with an optimum condition of maximum strength combined with maximum ductility at the Mo-35 pet composition. At higher rhenium contents, the ductility was severely impaired due apparently to the presence of brittle tetragonal s phase, Fig. 1. In the Mo-35 pet Re alloy, at least 110 ppm (parts per million) oxygen could be tolerated before cold workability was reduced. By comparison, the corresponding tolerance figure in unalloyed molybdenum is ~ 10 ppm. The effect of rhenium was considered in terms of: 1) a reduction in oxygen solubility in the lattice; 2) a redistribution of intergranular oxide from grain boundary films to isolated spheres; and 3) the promotion of twinning as a further mode of plastic deformation. Paradoxically, twinning is often associated with brittle fracture in iron and the silicon irons.6'7 Work to date has been restricted to are-melted and powder metallurgy polycrystalline material of ~ 99.9 pet purity. The present investigation was initiated for the purpose of determining the mode and crystallography of plastic deformation of a series of bee Mo-Re alloy single crystals over a wide temperature range from -196o to +200°C. Using high-purity zone-melted material (~ 99.99 + pet purity), the specific role of rhenium in the molybdenum lattice may be understood more fully since effects due to grain boundaries and oxide redistribution will be absent. At the same time, the study provides a comparison of single and polycrystalline deformation behavior. EXPERIMENTAL TECHNIQUES A) Preparation and Purity of Single Crystals. Alloys in the form of either are-cast and swaged or sintered and ground bar, 0.120 in. diam, were obtained from the Chase Brass and Copper Co. Alloy single crystals ~ 8-in. long were grown from the

Jan 1, 1962

By Milton E. Wadsworth, W. Martin Fassell, William H. Dresher

A study of the rate of dissolution of molybdenite (MoS2) in alkaline solution was carried out under carefully controlled conditions. Effects of temperature, oxygen over-pressure, and KOH concentration were evaluated. Studies were made in the temperature range 100°C to 175°C and in the pressure range 0 to 700 psia of oxygen. Under these conditions molybdenite was found to leach according to a linear mechanism. Both oxygen over-pressure and KOH concentration were found to control the rate of leaching. The mechanism has been explained in terms of adsorption of oxygen at the molybdenite surface followed by configurational rearrangement of the adsorbed molecules. The hydroxyl ion dependency is believed to be diffusion-controlled. Laboratory batch studies have shown that molybdenite can be readily dissolved in alkaline solutions under moderate conditions of temperature and pressure. Commercial application of this process to the production of ferro-molybdenum and molybdenum chemicals is promising in view of the ease of dissolution of molybdenite and the relatively noncorrosive conditions involved in the process. HIGH temperature-high pressure techniques have long been used to great advantage in the organic chemical industry, the petroleum industry, and the paper industry. Only recently, however, have these methods been used to extract metals from their ores on a commercial scale. The Chemical Construction Corp., together with interested producers of nickel and cobalt, has done much to develop methods of producing nickel and cobalt powders by the use of high temperature-high pressure techniques.' The Howe Sound Co. is currently operating a plant near Salt Lake City in which the new Chemical Construction Corp. technique is applied to cobalt-arsenic sulfide concentrates. In this method the concentrates are leached in a dilute solution of sulfuric acid under air pressure at a high temperature. Near Edmonton, in Alberta, Canada, the Sherritt Gordon Co. is also using the new method in conjunction with its ammoniacal leach process.' National Lead Co., at Fredricktown, Mo., is operating a process similar to that of Howe Sound. In spite of the rapid growth of high temperature-high pressure hydrometallurgical processes, there has been very little work done on fundamental principles involved in this type of process. Conse- quently the literature lacks any significant data in this field. Oxidation of pyrite,3 phalerite,4 galena,5 and recently molybdenite" in alkaline solutions has been reported to some extent. This investigation was initiated, therefore, to broaden the application of high temperature-high pressure hydrometallurgy and also to contribute some insight into the basic mechanisms of oxidation in an aqueous medium under these conditions. In addition to the immediate consequences of these processes much valuable information remains to be learned about fundamental reactions when they are carried out at temperatures and pressures slightly higher than those normally encountered. Leaching of molybdenite by alkaline solutions under oxygen pressure has recently been reported in the Russian literature by E. S. Usataya,8 who found that leaching rate increased with an increase in the pH of the solution—the strongest effects being observed at a pH of 10—and also with an increase in temperature. Usataya also has reported the formation of a protective film on the surface of the molybdenite when the leaching solution was weakly alkaline, neutral, or acidic. He believes that this oxidation process explains the migration of Mo+ + in the oxidation zones of molybdenite ore deposits and the subsequent impoverishment of the ores. Equipment: The high temperature-high pressure reaction unit used in this work was especially designed for kinetic studies of this nature, emphasis being placed on accuracy of measurement and precision of control. As details of the unit's construction and operation have been discussed elsewhere,7 Only basic features and principles of operation will be discussed at this point.

Jan 1, 1957

By F. C. Miller

THE metallurgical fuel of Colorado, Utah, and New Mexico has been a very tardy member in the caravan of western industrial progress. The history of western coke has naturally been closely related to the development of the metallurgy of iron and steel and the precious metals, in the State of Colorado. It was at Leadville, with a population of 300 in 1877, that the Sentinel was published by Richard S. Allen. The Sentinel gave very full accounts of the various mineral discoveries at the new town of Leadville, which found their, way to the more widely circulated journals of the East, and attracted the attention of many people. At the close of 1878, a census showed a total of 5040 persons. The first smelter was established in 1877, at Malta, two miles from Leadville, by A. R. Meyer, but was not successful. It was succeeded by the Harrison Reduction Works, in 1878. The La Plata began with one furnace in June, 1878, and in 1879 had four furnaces in active operation. These furnaces used charcoal for fuel, and, because of hot tops, suffered a tremendous loss in lead and silver. This difficulty was overcome by the erection of 50 single-bank 10-ft. beehive ovens at Crested Butte, Colo., in 1880. The slack coal sent to these ovens was very pure, and yielded a coke carrying as little as 4.5 per cent. ash. Among the pioneers in the Leadville district were Grant, Eddy, James, Billings, Eiler, and Dickson. To these men the West owes the present expansion of its mining industry, and the erection of metallurgical processes for the treatment of precious metals.

Jan 8, 1918

By H. C. Fiedler

It was recently shown with 3.3 pct Si-Fe containing 0.026 pct S and 0.06 pct Mn that the extent of secondary recrystallization to a cube-on-edge texture is determined by the cooling rate from the solution temperature of the manganese sulfide inclusions.1 With a rapid cooling rate, many small inclusions rather than a few large ones are formed, which leads to increased restraint to normal grain growth and more complete secondary recrystalliza-tion. Strip samples 12 mils thick, rolled from 1-in.-thick slabs that were cooled at 130°C per min

Jan 1, 1964

By B. Ramaswami, Y. Nakada, R. Schaefer

EARLY investigations1 of the tensile properties of fcc single crystals did not reveal the easy glide region of crystals with axial orientations inside the standard stereographic triangle. With the production of high-purity metal, a region of easy glide became known1 Consequently, modern work of fcc single crystals ordinarily uses high-purity metal. In order to determine whether further purification of aluminum beyond 99.992 pct purity would result in significant alteration of the tensile properties of single-crystal specimens, metal was zone-refined and crystals grown from the purified material were compared to crystals grown from the original material. Some similar studies were made of gold and silver crystals. Aluminum. The material to be zone-refined was cast into bars 1/4 by 1/2 by 8 in. A zone, approximately 1-1/2 in. in length, was passed over each bar eighteen times at a rate of 6 in. per hr. Melting and stirring were carried out by an induction heater under a vacuum of approximately 10"5 mm Hg, the metal being held in a graphite container. he last 3 in. of each processed bar were then cut off and discarded. No quantitative determination of purity was made, but the effectiveness of the zone refining was tested by a method first suggested by Walton, Tiller, Rutter, and winegard3 depending on the relation between cell structure and impurity content. Rutter and Chalmers4 have shown that a cellular substructure is associated with the presence of impurities during solidificatibn, and have shown how solute rejection at the freezing interface can lead to such an association. Thus the observation of cells gives evidence of impurities being present. To look for cells, the last quarter of a zone-refined bar was cut off, remelted, and grown rapidly into a single crystal. It was then heavily electropolished and thermally etched.~ Cells were revealed by the presence of many parallel rows of etch pits. The same process was carried out with material from the first half of the bar, but no cells were detected. These observations give evidence that a significant amount of impurity material was moved to the "dirty" end of the zone-refined bars. Further indication of purification was obtained from recrystallization experiments. It was found that, after cold rolling to a 97 pct reduction in thickness, the material from the pure end of the bar re-crystallized at room temperature, but the material from the "dirty" end did not. Other investigators6 have previously reported that zone-refined aluminum recrystallized at room temperature. The purified material was cast into 1/4 by 1/4 in. bars, and seeded crystals were grown in a (100) orientation and in a single slip orientation where the Schmid factor is m =2. The crystals were then cut to the desired length, annealed for 24 hr at 610°C, furnace-cooled, and etched in Tucker's etch. The crystals were tested in a floor-model Instron machine, using a gage length of 4 in. and a strain rate of 1/2 pct per min. The resulting curves are shown in Fig. 1. It is seen that the differences between the curves for zone-refined and original-purity materials are small. These differences are within the scatter observed for crystals of the original purity. In particular, the zone refining does not significantly affect the onset of the different "stages" of the curves.

Jan 1, 1964

By J. V. W. REYNDERS

NOT only is your toastmaster silver-tongued in his references 'to myself, but he is also quite in the habit of "saying it in silver." I have analyzed with some care his statistics of the world's silver production, which have been distributed here along with the menu, although frankly from the point of view of most of us, the distribution rather than the production of silver is of immediate concern. Unlike the performers by whom we have been entertained between courses, the rest of us on the program will have to do without costume or musical accompaniment, which as my friend Rains can testify puts an artist under severe strain. I am entitled by right of office and of precedent to receive your attention for ten minutes. The Governor, who appears on the program as a speaker; however, has asked me for five minutes of my time, and Senator Thomas has insinuated that he would appreciate one-half of the remainder, wherefore, I must ask your close attention to the very brief remarks that I am able to make under such restricted circumstances. To begin with, I want you to believe that I am approaching the task set by your toastmaster with misgivings. In looking over the Institute records relating to the Salt Lake City meeting of 1914 for some precedent as to what I ought to say, I found but one reference-and that of the following indefinite char¬acter-" and Friday night there was a hilarious banquet to 350 members and guests."

Jan 1, 1925

By D. C. Porterfield

-4s a result of world economic conditions brought about by the European war and the consequent loss of European markets for Venezuelan crude, production in Venezuela decreased from 205,433,000 bbl. in 1939 to 186,134,000 bbl. in 1940, or 9.4 per cent. This decline interrupted a steady annual increase in production from the country, which had been continuous since 1932. The Maracaibo Lake Basin in western Venezuela accounted for 135,738,000 bbl. during 1940, or 73 per cent of the total, as against eastern Venezuela's production of 50,396,000 bbl., or 27 per cent of the total for the country. Corresponding figures for 1939 were 167,688,000 bbl., or 82 per cent of the total from the Lake Basin, and 37,744,000 bbl., or 18 per cent from the east. These comparisons indicate the increasing importance of the newer developments in eastern Venezuela, but it is unlikely that production from the east will ever exceed that from the west. In all, 429 new wells were completed in Venezuela during 1940 as compared to 438 in 1939. Of the 1940 completions, 411 were in proved areas and 18 were wildcats; 389 (95 per cent) of the exploitation wells drilled were producers, I was a gas well and 21 were dry holes, while 6 (33 per cent) of the wildcats drilled were producers and 12 (67 per cent) were dry; 263 of the exploitation wells and 4 of the wildcats were in the Maracaibo Lake Basin and 148 exploitation wells and 14 wildcats were in the east, mostly in the State of Anzoategui. Exploration of the light-oil areas in the Tia Juana and Lagunillas fields was con- tinued during the year with favorable results. Along the lake shore, drilling was confined principally to fill-in wells in the La Kosa, Tia Juana, Laguni!las and Bachaquero fields, although some important semi-exploratory drilling was done in the Pueblo Viejo area between Lagunillas and Bachaquero fields. The only other developments of particular interest in the west were the successful completion of a step-out well lying to the south of the former southern limit of Mene Grande field, which adds considerable proved acreage to that field; and the failure of two wildcats that were drilled near the Colombian border to determine whether the productive sands of the Petrolea field in the Barco Concession, Colombia, extend into Venezuelan territory. In the east no new fields were discovered during the year, although five wildcats were completed as producers. Three of these, Guario No. I, Jusepin-56 and LM-I (Leona), discovered important extensions to previously proved areas and the remaining two, Cantos-I and SPN-I (Socororo), were subsequently proved to have tapped productive sands of small extent and operations in these areas have been suspended. The greatest activity in the east was concentrated in the Oficina field, where 105 new wells were completed during the year and production was increased from 22,540 bbl. per day during January 1940 to 57,627 bbl. per day during December 1940. Important development work was also done in the Jusepin. San Joaquin and El Koble fields.

Jan 1, 1941

By D. C. Porterfield

-4s a result of world economic conditions brought about by the European war and the consequent loss of European markets for Venezuelan crude, production in Venezuela decreased from 205,433,000 bbl. in 1939 to 186,134,000 bbl. in 1940, or 9.4 per cent. This decline interrupted a steady annual increase in production from the country, which had been continuous since 1932. The Maracaibo Lake Basin in western Venezuela accounted for 135,738,000 bbl. during 1940, or 73 per cent of the total, as against eastern Venezuela's production of 50,396,000 bbl., or 27 per cent of the total for the country. Corresponding figures for 1939 were 167,688,000 bbl., or 82 per cent of the total from the Lake Basin, and 37,744,000 bbl., or 18 per cent from the east. These comparisons indicate the increasing importance of the newer developments in eastern Venezuela, but it is unlikely that production from the east will ever exceed that from the west. In all, 429 new wells were completed in Venezuela during 1940 as compared to 438 in 1939. Of the 1940 completions, 411 were in proved areas and 18 were wildcats; 389 (95 per cent) of the exploitation wells drilled were producers, I was a gas well and 21 were dry holes, while 6 (33 per cent) of the wildcats drilled were producers and 12 (67 per cent) were dry; 263 of the exploitation wells and 4 of the wildcats were in the Maracaibo Lake Basin and 148 exploitation wells and 14 wildcats were in the east, mostly in the State of Anzoategui. Exploration of the light-oil areas in the Tia Juana and Lagunillas fields was con- tinued during the year with favorable results. Along the lake shore, drilling was confined principally to fill-in wells in the La Kosa, Tia Juana, Laguni!las and Bachaquero fields, although some important semi-exploratory drilling was done in the Pueblo Viejo area between Lagunillas and Bachaquero fields. The only other developments of particular interest in the west were the successful completion of a step-out well lying to the south of the former southern limit of Mene Grande field, which adds considerable proved acreage to that field; and the failure of two wildcats that were drilled near the Colombian border to determine whether the productive sands of the Petrolea field in the Barco Concession, Colombia, extend into Venezuelan territory. In the east no new fields were discovered during the year, although five wildcats were completed as producers. Three of these, Guario No. I, Jusepin-56 and LM-I (Leona), discovered important extensions to previously proved areas and the remaining two, Cantos-I and SPN-I (Socororo), were subsequently proved to have tapped productive sands of small extent and operations in these areas have been suspended. The greatest activity in the east was concentrated in the Oficina field, where 105 new wells were completed during the year and production was increased from 22,540 bbl. per day during January 1940 to 57,627 bbl. per day during December 1940. Important development work was also done in the Jusepin. San Joaquin and El Koble fields.

Jan 1, 1941

By P. A. Beck, M. V. Nevitt

All binary and a number of ternary u alloys formed by first long period transition elements were examined and found to be ferromagnetic at low temperatures. The Curie temperatures for these alloys were measured. It was found that the correlation of the Curie temperature with composition may be described qualitatively in terms of the contributions of the various component atomic moments to the saturation moment of the alloy. Ternary Fe-Cr-Mo u phase alloys were also found to be ferromagnetic, with a Curie temperature dependent on the iron content and largely independent of the unit cell dimensions. Similar relations were found for the Co-Fe-Cr and the Co-Cr-Mo a alloys, where the Co + Fe content appears to determine the Curie temperature. RECENTLY, it has become increasingly evident that the u phase is some kind of an "electron compound." Several papers1-' discussed the empirical correlation between the composition of the various u phases in alloys of the transition elements and the distribution of electrons in the partially filled d-levels of the component atoms. However, a picture of the latter can be formed only in a more or less intuitive manner, as in the Pauling theory," and the rigorous treatment of these problems is at present prevented by lack of adequate knowledge of the electronic structure of the transition elements in the metallic state. It appeared reasonable to expect that investigation of the magnetic properties, which are related to d-shell electrons, may help in clarifying the physical nature of the foregoing empirical correlation. Qualitative tests of samples of various compositions have shown that certain u alloys become ferromagnetic at liquid nitrogen temperature." The present investigation was undertaken to determine whether or not low temperature ferromagnetism is characteristic of a large variety of u alloys and to establish how the Curie temperatures of ferromagnetic u alloys are influenced by changes in composition and in lattice parameter. In the first portion of the in- vestigation, Curie temperatures were measured for a series of u alloys containing either vanadium or chromium with one or two of the elements manganese, iron, cobalt, or nickel. In the second phase of the work, data were obtained on the Curie temperature of ternary (Fe, Co, Cr)a, (Fe, Cr, Mo)a, and (Co, Cr, MO)U alloys, as a function of composition and of interatomic spacing. Experimental Procedures High frequency vacuum melting in high purity re-crystallized alumina crucibles was employed in the preparation of the u alloys, using metals whose lot analyses are given in Table I. Approximately two-thirds of the alloys were analyzed chemically, the analytical results being in acceptable agreement with the intended compositions, as seen in Tables I1 and 111. The specimens were annealed for homogen-ization in an atmosphere of purified 92 pct He and 8 pct H, mixture or in evacuated and sealed Vycor tubes at temperatures from 780" to 1300°C, depending on the temperature range of the u phase field for the particular composition. The annealing temwerature and time for kach alloy are given in Tables 11 and 111. Curie points were determined by an induction method; the change with temperature of mutual inductance between two coils was observed when the i-u specimen was inserted into the flux path between the coils. The transformer consisted of three coils each containing 1200 turns of 0.0050 in. diam enameled copper wire. The center coil, P in Fig. 1, served as the primary coil, and was linked magnetically with each of the two secondary coils, S, and S? which were connected in series opposition. The primary coil, P, was energized by an audio-oscillator, set at a frequency of 500 cycles per sec, while the signal from the transformer secondary circuit,

Jan 1, 1956