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By H. W. Highriter

THE method developed and used in this laboratory for the production of metallic uranium of such purity that it is ductile and can be cold-worked to fine wire or thin sheet by rolling has already been described1. It consists, briefly, in the electrolysis of potassium uranous fluoride (KUF5) in a molten bath composed of equal parts of sodium and calcium chlorides. The bath is contained in a graphite crucible, electrically heated to about 775° C., the crucible serving as the anode for electrolysis. The uranium deposits in finely divided form mixed with salts upon a molybdenum cathode suspended axially in the crucible. Upon com-pletion of the electrolysis the cathode is removed and cooled, the deposit broken and leached to remove salts. The metal powder is washed with water and dilute acetic acid and dried in vacuo to reduce oxidation. Suitable amounts are then pressed into pellets and heated in vacuo by high-frequency induction, using a thoria crucible. The uranium melts and flows away from the pellet, leaving a shell, which is largely oxide. In general, this method produced a satisfactory metal, although at times the uranium was not ductile. The investigations recorded here were made to find the cause of this embrittlement. It was known that the metal generally contained carbon, derived from disintegration of the graphite crucible in which electrolysis is conducted, in amounts dependent upon the thoroughness of washing the metal powder. Accordingly, analyses of several samples, both ductile and brittle, were made by combustion and absorption of C02 in Ascarite, using air instead of oxygen to reduce the temperature and rate of oxida-tion. Several of these metals were made with special precautions to reduce carbon content. The results show no relationship between ductility and carbon content in the range investigated (Table 1).

Jan 1, 1935

By Dan Chun

Abstract-To facilitate the efficient handling of large volumes of information generated by logging exploration drill cores, a computer data bank system (GEOBANK) has been developed to store and retrieve the normally difficult to handle geologic information as well as the physical testing data. The data bank systematized the logging of drill core by first developing a standard list of adjectives or descriptors (with the corresponding assigned numerical codes) for the various stratigraphic categories that are also assigned numerical codes. The system uses the "floating-slot" concept and handles the data bank with one single input form.

Jan 9, 1978

By W. J. Taylor

SOME eight years ago I became interested to a considerable extent in one of the well-known deposits of sulphury iron ore in New Jersey, and, as a consequence, soon became interested in the subject of the elimination of the sulphur. On investigation I found that no department of pig-iron manufacture had received less attention than that of roasting or calcining ores for the elimination of sulphur, carbonic acid, water, etc. My first devices to eliminate sulphur were naturally in the lime-kiln line, with solid fuel mixed with the ore, in the same way as common lime is burnt with small coal. While this process will succeed tolerably well for carbonates or calcareous ores, even though they contain sulphur as sulphates, I soon found it would not answer for our magnetites, which are very hard and dense, carrying from 2 to 5 per cent. of sulphur as pyrites, and become very sticky as soon as any attempt is made to roast them at a high heat. Some laboratory experiments developed the fact that the nearer the gaseous current surrounding the hot ore approached in composition pure atmospheric air the more rapidly the sulphur was oxidized, while in an atmosphere composed largely of carbonic oxide, carbonic acid, and nitrogen, it seemed almost impossible to reduce the sulphur more than one-half, which was a confirmation of the well-known fact that just one-half of the sulphur in pyrites volatilizes very easily, and that the trouble is mainly to remove the remainder. It was thus apparent that the atmosphere surrounding the ore was of as much importance as the temperature. This led to the trial of a kiln to heat the ore by conduction through the brick. It was divided into ore-chambers, which were surrounded with flues, through which the products of combustion of gaseous fuel passed without coming in contact with the ore. We did not, however, succeed by this arrangement in getting more than a cherry-red heat, which, of course, was too low to accomplish anything. I had at this point become convinced – 1st. That gaseous fuel only would accomplish the work successfully. 2d. That since a high temperature was required to insure a rapid oxidation of the sulphur, and also to make the ore open and porous,

Jan 1, 1881

By W. J. Taylor

Some eight years ago I became interested to a considerable extent in one of the well-known deposits of sulphury iron ore in New Jersey, and, as a consequence, soon became interested in the subject of the elimination of the sulphur. On investigation I found that no department of pig-iron manufacture had received less attention than that of roasting or calcining ores for the elimination of sulphur, carbonic acid, water, etc. My first devices to eliminate sulphur mere naturally in the limekiln line, with solid fuel mixed with the ore, in the same way = common lime is burnt with small coal. While this process will succeed tolerably well for carbonates or calcareous ores, even though they contain sulphur as sulphates, I soon found it would not answer for our magnetites, which are very hard and dense, carrying from 2 to 5 per cent. of sulphur as pyrites, and become very sticky as soon as any attempt is made to roast them at a high heat. Some laboratory experiments developed the fact that the nearer the gaseous current surrounding the hot ore approached in composition pure atmospheric air the more rapidly the sulphur was oxidized, while in an atmosphere composed largely of carbonic oxide, carbonic acid, and nitrogen, it seemed almost impossible to reduce the sulphur more than one-half, which was a confirmation of the well-known Pact that just one-half of the sulphur in pyrites volatilizes very easily, and that the trouble is mainly to remove the remainder. It was thus apparent that the atmosphere surrounding the ore was of as much importance as the temperature..• This led to the trial of a kiln to heat the ore by conduction through the brick. It was divided into ore-chambers, which were surrounded with flues, through which the products of combustion of gaseoua fuel passed without coming in contact with the ore. We did not, however, succeed by this arrangement in getting more than a cherry-red heat, which, of course, was too low to accomplish anything. I had at this point become convinced— 1st. That gaseous fuel only would accomplish the work successfully. 2d. That since a high temperature was required to insure a rapid oxidation of the sulphur, and also to make the ore open and porous,

Jan 1, 1881

By W. Evans, C. E. Ells

The agglomeration of hydrogen in pure aluminum and A1-Mg alloys has been studied through use of hydrogen introduced into the metal by cyclotron proton irradiation. Both the growth and dispersal of the agglomerates have been followed by metal-lographic techniques. During the cyclotron irradiation, agglomeration occurs at temperatures i 100°C for hydrogen concentrations as low as 1 ppm. On heating at elevated temperatures, 300°C to 600°C, intragranular agglomerates first coarsen and then disperse. The agglomerates formed at grain boundaries are much larger than the intragranular agglomerates; with hydrogen concentra- tions > 10 PPm, heating for 1 hr at 500°C results in extensive grain-boundary cracking. The hydrogen agglomerates have been shown to inhibit grain growth, but no inhibition of recrystallization has been observed. The ability of hydrogen to enter aluminum at a free surface, combined with its high-diffusion rate at elevated temperatures, accounts both for growth and dispersal of the agglomerates. Irradiations at elevated temperatures give results consistent with the explanation proposed for agglomerate behavior on post-irradiation heating. 1 HE formation of hydrogen-filled bubbles, or blisters. in aluminum and its alloys has been studied for over' thirty years. The work up to 1952 has been reviewed by Kostron' and since then Ransley and

Jan 1, 1963

By Harry H. Power

WHILE the attention of all engineering branches is focused today on changes and improvements in the several curricula, we are concerned here with the many questions arising in industry and college concerning the preparation for the petroleum engineering profession. The succession of problems confronting the petroleum engineer demands a degree of versatility not ordinarily encountered in other professions. As a consequence, the student cannot acquire mastery of all the several engineering branches represented in field practice, and as an alternative, he has learned to appreciate the value of thorough training in the basic or fundamental sciences as a preliminary foundation for professional work. While our attention is directed primarily to the training of engineers in educational institutions, it is necessary that the ultimate education of the professional engineer be kept in mind. It is apparent that his success as an engineer is limited not only by his educational and job experience, but by his native endowments: mentality, personality and health. The engineer's lack of job experiences often proves as much a handicap as the lack of adequate college training. If the final product proves to be satisfactory, both industry and technical institutions are to be congratulated. However, if the product is found wanting, the one most responsible should be apprehended. FITNESS FOR PROFESSION For the most part, students of engineering colleges have had their interests in applied science awakened at a relatively early age. Many of them entered college as a convenient means of acquiring a technical education, but undoubtedly would have had better prospects in a shorter program offered by institutions of noncollege grade. The activating motive of practical interest is also strong in students suitable for college training, but in many cases an intellectual interest must be awakened in order that it may survive graduation. Numerous engineers believe that this progressive process of selection and determination of career aims is one of the essential services rendered by the engineering colleges. Industrialists, who are more interested in quality than quantity of petroleum engineering graduates, have pointed out the good that should result if more emphasis were given to the work of eliminating the misfits. They also point out the protective measures that have been taken by other professions for the betterment of professional standards. Mention has been made of the beneficial results to be obtained by collective determination of the market for the products of engineering schools, particularly in that the students unsuited to the profession would have an opportunity to prepare themselves for employment more suited to their personalities and other qualifications. In the event that such a system of coordinated personnel direction is developed by the

Jan 1, 1941

By E. O. Jones

DURING the heating of cold-worked nickel silver, the tendency of the material to crack is well known. The present research deals with this question, and may conveniently be divided into the following sections: Changes in these alloys during heating and cooling, determination of the temperature at which cracking occurs, effect of grain size, quenching cracks, methods of overcoming annealing cracking. The work is far from complete, in particular the influence of impurities on this tendency has not been investigated, but the results so far obtained lead to certain definite conclusions, which are of theoretical and practical importance. CHANGES IN ALLOYS DURING HEATING AND COOLING During the annealing of many metals at a temperature just below that at which recrystallization sets in, there is evidence of some change, the effect of which is to harden and embrittle the material. This effect has been most clearly demonstrated in the cases of aluminum, copper, brass, and nickel silver, and appears to be a common property of cold-worked metals and alloys, or, at any rate, the non-ferrous ones. The effect would obviously offer an explanation for certain types of annealing cracking, but the trouble is so much more common in the nickel silvers than in the other alloys that some special cause should be looked for. There is, however, fairly good reason for believing that similar cracking may occur in some of the brasses; D. Bunting suggests that the a brasses toward the saturation limit are subject to a transformation closely allied in nature to that known to occur in the nickel silvers at around 320° C. Although the existence of this critical temperature range was known, it did not necessarily follow that this transformation was responsible for the trouble under investigation, so the first portion of this paper deals with the attempts made to determine whether other critical changes might not occur in these alloys. There were already reasons for the belief that such would prove to be the case, as the mechanical properties of the nickel

Jan 7, 1925

J. M. HARTMAN, Philadelphia, Pa.: Mr. Fackenthal can remember some queer things that occurred at Durham, Pa., Aug. 3, 1876, while he was superintendent. The furnace was working stiff, i.e., blast-pressure 10 to 11 pounds, which was high pressure for those days. With this pressure there was some circulation through the stock. At 9 p.m., flushed cinder. After flushing, air was thrown off' for a moment to " bot up "; the keeper turned the lever and threw on air just as the scaffold dropped, which eased up the pressure to 4¼ pounds. The air-receiver is twice as large at Durham as at other places. The air from this receiver, added to the two seven-foot blowers, gave an extra large volume, which, rushing into the furnace, fired the finely-divided carbon, causing an explosion that threw part of the stock in the furnace out into the open air, threw up the bell-and-hopper with the tunnel-head plates, and gave off' a large volume of carbondust. The bell-and-hopper going up first, the stock followed, and, striking the bell-and-hopper, was deflected in a shower over the cast-house roof, breaking the slates. Sitting at the corner of the engine-house at the time, the stock pelted me, when I ran around the corner to get rid of it. Remembering there were two men at the furnace-top, I shut down the engines, and, running to the top, found them sitting in the hoist-house enjoying the fire-works. The explanation of this explosion is simple. There is in the blast-furnace a bed of fuel extending up, say, 16 to 18 feet above the tuyeres; in this bed of fuel some stray pieces of limestone are found, and a few pieces of unreduced ore; but, generally speaking, it is all fuel. On this bed of fuel is the zone of fusion. In this zone the descending stock is liquefied, except the fuel; the iron, melting, drops out of the ore, and the gangue unites with lime, forming cinder. The iron falls in the form of shot, and, with the cinder, trickles

Jan 1, 1899

By S. E. Bretherton

Discussion of the paper of S. E. BRETHERTON, presented at. the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1595 to1599. ANTON EILERS, Brooklyn, N. Y. (communication to the Secretary*). While the advantages in the use of high-line siliceous slags in lead smelting which Mr. Bretherton discusses in this paper are obvious under certain economical conditions, he gives me credit for the introduction of such slags when it does not belong to me. It is true I did considerable experimental work, off and on, for the purpose of finding such slags, while at the Germania in 1877 and 1878, but I did not have occasion to introduce any such slags for regular work, because I had no ores which fitted the economical conditions for using high silica and high lime, except in isolated cases for very brief periods. On the contrary, the ores I had to treat were mostly very ferruginous and very low in silica, so that, economically, I was compelled to run nearly always on slags, which allowed me to use the abundant flux I had without cost. It was August Raht who first had occasion to establish and use for long periods a slag high in silica and line, and low in iron. This was when he was confronted with the task of smelting the. Horn-Silver ores at the smelting works at Franklin, Utah, with as little expenditure for fluxing material as possible. I was at that time in Leadville, Col., where, in the new works I had built, the Billings and Eilers smelters, I had occasion to use profitably many slags, but never anything as high in the earthy bases and in silica as Mr. Raht had to use.

Jan 12, 1915

By J. P. Neumann, Y. A. Chang

Lattice parameter measurements of the hcp phase in the system Ag-A1 near the stoichiometric composition Ag2Al were carried out for specimens quenched from 825°K, annealed for 10 days at 453°K, and annealed for 100 days at 413°K. The three heat treatments resulted in the same lattice parameters at room temperature. None of the specimens showed any superlattice lines. The lattice parameters of this alloy were also measured at temperature from 77° to 750°K. An anomaly in the temperature variation of the lattice paramete.rs occurs in the region near 400°k, which may be associated with local ordering. FROM measurements of the diffuse scattering of X-rays, it is known that the [ phase in the system Ag-A1 near the stoichiometric composition Ag2A1 ex- hibits a considerable degree of short-range order at room temperature.' Moreover, based on the position of the short-range order peaks a superlattice model had been proposed in the same study and it was suggested that lowering the annealing temperature to 420°K might result in long-range order. In the present study, the diffraction patterns and the lattice parameters of three differently heat-treated specimens, i.e., quenched from 825°K, annealed for 10 days at 453°K, and annealed for 100 days at 413°K, were determined from 77" to 750°K. The purpose of these measurements was to investigate 1) whether long-range order could be established by prolonged annealing and 2) whether the lattice parameters at room temperature depended on the heat treatment, since it had been proposed earlier2 that the lattice parameters in this phase are related to the atomic arrangement. 1) EXPERIMENTAL TECHNIQUES Silver and aluminum, both 99.99 pct purity, were melted in a zirconium oxide crucible under helium in

Jan 1, 1969

F. N. SPELLER (communication to the Secretary*).-It would certainly be interesting to know more about the heat balance in this practice, but there seems to be no doubt that the net result is a greater absorption of heat where roll scale is used instead of solid metal scrap. In the experimental heats referred to, about an equal weight of pig iron or steel scrap was replaced by roll scale. This caused a reduction of about one-third in the time of blow compared with a heat of the same

Jan 6, 1917

By J. D. Kalasky

Continuous mining has revolutionized the coal industry but intensified the problems of earlier mechanization. From the installation of the first miner, it was recognized that face ventilation would be one of these problems. To establish an efficient work cycle for the equipment being used, conventional mechanized mining provides four or more development faces. Continuous mining, relying on a single machine, requires only one face, although more than one can be driven alternately by the same machine. In gaseous areas mined by the older methods, the intermittent rate of exposure allows time for the face to bleed off or be cleared, and the width obtained with conventional units makes it possible to hang a brattice line almost to the face. Continuous mining increases the ventilation hazards; there is no margin of time, and very limited space. For all practical purposes, continuous miners available today can be grouped into two major types, rippers and borers. The two can be further classified, respectively, as flexible and rigid. Both types have been in operation in U. S. coal mines for the past five to ten years in a number of seams, under various conditions ranging from slightly gaseous to very gaseous. Common methods of face ventilation utilizing jute or plastic brattice material for line curtains, stoppings, and checks have so far met with success. Air volumes to operating sections are greater than for conventional mining, and specific instructions have been given to section crews stressing the precautions needed in dealing with a steady rate of gas emission and the importance of maintaining reasonably air-tight brattice to direct a good steady flow toward the face at all times. Operators of continuous miners, as well as the foreman on each section, are equipped with an approved safety lamp for gas testing. When the miner is in steady operation, tests for gas at the face are made at 15 to 30-min intervals, depending on the

Jan 1, 1960

By Mohamed Mortada

A practical analytical method is developed in this paper which provides the practicing reservoir engineer with a handy method for analyzing oilfield interference problems. The procedure employed entails the principle of superposition of individual eflects. A set of charts has been developed and can be used to evaluate the individual effects. The charts represent non-steady state pressure distribution in an extensive aquifer due to a constant rate of production from an oilfield which can be approximated by circular geometry; they are constructed from solutions to the diffusivity equation considering a circular sink as distinguished from a point sink. The solutions are obtained partially from mathenlatical considerations and partially from analog and digital computations. By virtue of the method of images, the charts can be used also to treat the case of production near a fault. In addition, provisions are made for treating oil fields, which are produced by partial water-drive. Treating an actual field case is deferred to a subyequent writing; however, illustrative example is presented to demonstrate the method of application. The pressure distribution in linear and limited radial aquifers is currently under study. INTRODUCTION With the increasing difficulty of discovering new oil reserves, attention is necessarily focused on the efficient development and production of existing reservoirs. Efficient production depends on the availability of reliable means for predicting the pressure-production behavior of oil fields. The prediction is usually performed by analytical methods or computers. Analytical methods are often limited to systems which can be approximated by simple geometry. However, analytical methods have the distinct advantage of being readily performed without special equipment. Analog and digital computers lend themselves to a variety of problems, but are not always locally available and consequently their use is limited. One particular situation in which analytical techniques are needed involves studies of multiple, water-drive oil fields sharing a common aquifer. Such oil fields are in hydrodynamic communication. Therefore, production from any of the oil fields is accompanied by a pressure decline which is transmitted through the aquifer to the other oil fields and manifested as pressure interference. The rate of propagation of the pressure decline is such that the pressure may be significantly reduced many miles away from a producing pool. An example of pressure interference is found in the Woodbine formation in East Texas. There. a dozen or more pools, including several of major size, draw on the Woodbine formation for water drive. The pressure in the water-bearing portion of the formation has been significantly reduced over an area of several thousand square miles. This reduction of pressure has been such that when the Hawkins pool was discovered in 1940, the pressure in it had already been reduced 280 psi below the initial value in the aquifer. This resulted from prior production from other Woodbine sand pools, including, in particular, the East Texas field some 20 miles to the east of Hawkins.' The above example indicates that the interference effect can be significant and should be taken into con-

Jan 1, 1956

By V. F. Parry, E. O. Wagner

This paper summarizes investigations during 1949 on three pilot plants for drying low-rank fine coal by entrapment in hot gases. Detailed operating results on processing seven coals having moisture ranging from 24 to 62 pet, formulas and data for calculating performance of large units, and general conclusions on the problem of drying fine coal are presented. THIS paper presents a summary of investigations by the Coal Branch of the Bureau of Mines during 1949 on the removal of internal moisture from low-rank coals by processing them in the entrained and fluidized state. A paper on this subject, giving a summary of the early work, was presented at the 1949 AIME annual meeting1 and gave a the- oretical discussion of the time and heat required to dry various sizes of low-rank coal. The investigations on two pilot plants were presented in the foregoing paper. During 1949, three additional pilot plants were built to study phases of the drying problem and to investigate different techniques of handling fine coal in the entrained and fluidized state. The present paper gives operating data on the new units and presents detailed data on the drying of seven coals having bed moisture ranging from 62 to 24 pct. The problem of removing surface moisture from fine coal is principally one of heat exchange and dispersion of the coal particles so that heat can reach the liquid moisture to permit evaporation, and it does not involve the factors of size and time of contact to any great extent. If enough heat can reach the surface of the particles at temperatures higher than 250°F, moisture evaporates almost instantly, and the factors of time and size are of secondary importance compared with the factors of heat balance and dispersion of the coal. Therefore, it does not appear to be necessary to employ a fluidized bed when removing surface moisture, and the most efficient process would be one in which the coal particles are entrained in a hot gas stream of optimum temperature traveling at a velocity that causes the particles to disperse into a low-density phase. When low-rank coals are dried, the fluidized bed is necessary to provide control of time of contact. This is done by adjusting the superficial velocity which controls the density or dispersion of the particles. The density of beds having fluidized properties suitable for drying low-rank coals appears to range from about 5 up to about 15 lb per cu ft. When the density is below 5 lb per cu ft, which represents a low-density phase, optimum conditions for removal of surface moisture should be found, and this requires superficial velocities of about 15 fps. The problem of removing bed moisture from low-rank coals involves consideration of size of coal, temperature, mass flow, heat balance, pressure, time of contact, and method of dispersing the coal in the heating mediums. The experimental work presented here gives data on these factors. Coal sizes up to 1/2 in. x 0 were dried with hot gases having initial temperatures ranging from 1900° to 2400°F. Coal

Jan 1, 1951

By E. O. Wagner, V. F. Parry

This paper summarizes investigations during 1949 on three pilot plants for drying low-rank fine coal by entrapment in hot gases. Detailed operating results on processing seven coals having moisture ranging from 24 to 62 pet, formulas and data for calculating performance of large units, and general conclusions on the problem of drying fine coal are presented. THIS paper presents a summary of investigations by the Coal Branch of the Bureau of Mines during 1949 on the removal of internal moisture from low-rank coals by processing them in the entrained and fluidized state. A paper on this subject, giving a summary of the early work, was presented at the 1949 AIME annual meeting1 and gave a the- oretical discussion of the time and heat required to dry various sizes of low-rank coal. The investigations on two pilot plants were presented in the foregoing paper. During 1949, three additional pilot plants were built to study phases of the drying problem and to investigate different techniques of handling fine coal in the entrained and fluidized state. The present paper gives operating data on the new units and presents detailed data on the drying of seven coals having bed moisture ranging from 62 to 24 pct. The problem of removing surface moisture from fine coal is principally one of heat exchange and dispersion of the coal particles so that heat can reach the liquid moisture to permit evaporation, and it does not involve the factors of size and time of contact to any great extent. If enough heat can reach the surface of the particles at temperatures higher than 250°F, moisture evaporates almost instantly, and the factors of time and size are of secondary importance compared with the factors of heat balance and dispersion of the coal. Therefore, it does not appear to be necessary to employ a fluidized bed when removing surface moisture, and the most efficient process would be one in which the coal particles are entrained in a hot gas stream of optimum temperature traveling at a velocity that causes the particles to disperse into a low-density phase. When low-rank coals are dried, the fluidized bed is necessary to provide control of time of contact. This is done by adjusting the superficial velocity which controls the density or dispersion of the particles. The density of beds having fluidized properties suitable for drying low-rank coals appears to range from about 5 up to about 15 lb per cu ft. When the density is below 5 lb per cu ft, which represents a low-density phase, optimum conditions for removal of surface moisture should be found, and this requires superficial velocities of about 15 fps. The problem of removing bed moisture from low-rank coals involves consideration of size of coal, temperature, mass flow, heat balance, pressure, time of contact, and method of dispersing the coal in the heating mediums. The experimental work presented here gives data on these factors. Coal sizes up to 1/2 in. x 0 were dried with hot gases having initial temperatures ranging from 1900° to 2400°F. Coal

Jan 1, 1951

By S. G. Proctor, D. L. Baaso, W. V. Conner

A double crucible system was developed for I-g scale plutonium reductions. The equipment consists of an inner MgO crucible, an outer MgO crucible, and a stainless steel pressure vessel. The reduction charge is PIaced in the inner crucible and the annulus between the inner and outer crucibles is filled with a mixture of calcium and iodine. The exothermic reaction between the calcium and iodine in the annulus supplies the heat required for complete reaction of the reduction charge ana' good metal coalescence. Metal yields of 80 to 85 ,pct were obtained from I-g scale reductions and yields as high as 97.5 pct were obtained from 0.5-g scale reductions. The system was used to reduce charges containing as little as 0.1 g of Pu resulting in metal yields up to 90 Pct. THIN metal foils of highly enriched plutonium isotopes are used as targets for cross section and other measurements. The isotopes are separated in the calutrons at Oak Ridge and are very expensive to prepare. Often, only 1 or 2 g of material are available thereby emphasizing the need for a method of preparing these small quantities of metal. Procedures for 1-g scale plutonium reductions have been described, but these procedures require elaborate or expensive equipment. For example, the procedure described by Anselin et al.1 requires an inert atmosphere glovebox and induction heating equipment. The procedure described by Baker2 also uses induction heating equipment to obtain the recommended heating rates and liner temperatures. Baker's procedure also requires high purity PuF4 with very little PuO2 present. The procedure described in this paper resulted from a search for a simple and inexpensive method for making 1-g scale plutonium reductions. EXPERIMENTAL Equipment. The equipment required for the double crucible system consists of a pressure vessel, two MgO crucibles, a MgO crucible lid, and a resistance-heated, vertical crucible furnace. The crucibles were slip cast from high purity MgO and were supplied by the Coors Porcelain Co. and the Norton Co. The pressure vessel and lid were fabricated from 316 stainless steel. Materials. The PuF4 used for this study was obtained from the P1utoniu:m Metal Production Department at Rocky Flats. The PuF4 was prepared in a con- tinuous hydrofluorinator by reacting Pu02 with HF at 650°C. The isotopic composition of the plutonium was approximately 93 pct 239PU, 6 pct 240PU, and 0.5 pct 241PU. Some of this PuF, contained less than 1 pct Pu02 (Batch No. 6 and 7), while other batches contained up to 15 pct Pu02 (Batch No. 3). The chemical analyses of all the PuF4 used for this study is given in Table I. The calcium was 99 pct pure, AEC grade, and only that fraction which would pass through a 20 mesh screen was used. The I2 was USP grade re-sublimed I2 which was ground before being used. Procedure. Various charge compositions and methods for loading the double crucible system were tested. The optimum conditions for 1-g scale reductions are described below. The double crucible system was loaded as shown in Fig. 1. The outer crucible was placed in the pressure vessel and the annulus between them was filled with MgO sand. The inner crucible was placed in the outer crucible, supported by a layer of MgO sand in the bottom of the outer crucible. A mixture of 5.2 g of Ca and 25 g of I2 was placed in the annulas between the two crucibles. The upper portion of the annulas was filled with MgO sand. Next, a layer of a mixture of calcium and I, equal to 20 wt pct of the calcium and I2 used in the main charge was placed in the bottom of the inner crucible. The PuF, to be reduced was mixed with a 30 pct excess of calcium and 1 mole of I2 per mole of Pu and this mixture was placed in the inner crucible. The charge was topped with a layer of a mixture of calcium and I2 equal to 20 wt pct of the calcium and I2 used in the main charge. The pressure vessel was sealed with a flat copper gasket and was purged by alternately evacuating and filling with argon. The purge valve was closed and the vessel was placed in a vertical crucible furnace which was preheated to 950°C. The furnace was turned off after 20 min of heating and the vessel allowed to cool. Experience has shown that. this amount of heating is sufficient to assure complete reaction of the charge. RESULTS AND DISCUSSION The double crucible system has been used to produce plutonium metal on a 0.1- to 1-g scale. Reduction

Jan 1, 1970

By Appendix by A. S. Goldoni, R. E. Tate, E. M. Cramer

The diffision coefficient for self-diffision of plutonium in the temperature range 350" to 440°C has been measured by using puZ3 as the tracer isotope. Autoradiopaphic techniques were used to inzlestigate the possibility of grain boundary diffusion, hut only evidence for volume diffusion was found. The least-squares fit of the data gives the .following equation for the diffision coefficient: The computer least-squares technique for fitting the nonlinear equations is outlined. DETERMINATION of the self-diffusion coefficient of the fcc 6 phase of plutonium is in principle a straightforward experimental task. However, the chemical reactivity, the intense @ activity, and the toxicity of plutonium put limitations on the experimental techniques. The technique selected included roll bonding for preparation of the diffusion couples and pulse-height analysis of the @-particle activity to determine the distribution of the PU tracer in the diffusion couples. EXPERIMENTAL PROCEDURE Couple Preparation. Cylinders about 0.5 in. in diam were cast from two special stocks of plutonium, one of which had been enriched in puZ3', as shown in the isotopic analyses listed in Table I. For each roll-bonded composite sheet, a cylinder 0.437 in. in diam and 0.190 in. thick was turned from each kind of plutonium on a lathe in a 98 pct He atmosphere. The two freshly machined cylinders were positioned face to face in a tube of commercially pure aluminum which had been sealed at one end by welding and the assembly was evacuated on a vacuum manifold overnight. The elapsed time between machining the faces of the plutonium cylinders and evacuating the loaded tube was about 15 min. After overnight evacuation of the assembly the indicated vacuum was 1 X 10"5 torr or better. The aluminum tube was then warmed and pinched off with a cold-welding tool. The pinched-off weld was also fusion-welded as an additional precaution against leakage of air into the evacuated assembly. The assembly was immediately heated for 30 min in a 250°C furnace and reduced in thickness by being passed through a rolling mill with rolls heated to 200°C. The rolling schedule (four passes of 100 mils each with a 10-min reheat after two passes) reduced the thickness of the assembly to 100 mils. The rolled assembly was allowed to cool normally in air. The rolled assembly was sheared at the edges and the aluminum peeled from the composite plutonium sheet. The elliptical sheet was about 0.060 in. thick and usually three 0.383-in.-diam disks could be punched from its central portion. The sheet was heated on a hot plate to the ductile low 0 range (140°C as measured by temperature-indicating pellets) before each disk was quickly punched. The quality of the bond in the disks was evaluated by metallographic examination of the scrap sheet adjoining the hole left by the punch. Only well-bonded specimens without oxide in the interface (as indicated by metallography) were considered satisfactory for further use. More than half of the specimens so examined contained sufficient oxide in the interface to be rejected. Diffusion Anneal. Each disk to be diffusion-annealed was wrapped in 1-mil-thick tantalum foil and sealed within a Pyrex capsule evacuated to 1 x 10~5 torr or better. This capsule was then sealed within another Pyrex capsule at a similar pressure. The diffusion anneals were carried out at temperatures between 350" and 440°C in Marshall furnaces adjusted to have a temperature gradient of not more than *1/2"C over a 5-in. length. This gradient was then further smoothed by using a nickel tube as a liner in the furnace. The liner was divided into three longitudinal cavities by a septum of nickel sheet to which two calibrated Chromel-Alumel thermocouples were attached. One thermocouple was used for controlling the furnace temperature by means of a Brown Pyrovane controller equipped with a Capaciline anticipation circuit; the second thermocouple was monitored twice daily with a Leeds and Northrup K-2 precision potentiometer.

Jan 1, 1964

By Sterling G. Valentine

The annual .use of large quantities of sulphurous iron-ores (over 1,500,000 tons in the United States) has led to a search for the best methods of desulphurization, in order to make this material more available for the manufacture of a good quality of pig-iron. Although such ores can be used raw in small amounts, they must be previously roasted if they are to constitute the entire ore-charge of a furnace.

Jan 1, 1890

By Richard Kunter

INTRODUCTION Additional work has been done on the CIP circuit at Creede, and a brief description of this work is presented in this paper. DREDGE The original dredge for the Bulldog was built by Al Hack, Inc. of Denver. The dredge cutter head is mounted on a boom made of 6-inch diameter pipe which is raised and lowered by a cable-pulley system. Maximum cutting depth is 8 feet. Slurry from the dredge flows through a floating 6-inch diameter pipe supported on 55-gallon drums which runs from the dredge to the shore and then to a trash screen and pumping system. See Figures 1 and 2. The cutter head, suction pump, winches for dredge movement, and all other operations are controlled from a small operations house located toward the rear of the dredge. All of the basic dredge equipment is mounted on a chassis about 8 ft x 16 ft in size. Additional buoyancy was originally provided by sealed 55-gallon drums supported along the sides of the chassis by a small wooden framework. Additional framework and barrels on the front of the chassis on either side of the cutter boom provided additional stability, particularly when digging in hard material. The dredge was quite stable, but two problems were apparent. For one, it could have been sunk by someone from the shore firing a rifle into all of the barrels. In prime deer-hunting and sportsman country

Jan 1, 1983

By P. R. Celmer, Leonard R. Weisberg

THE principle of fractional crystallization has been successfully used to prepare high-purity (99.999 pct) Ga. Hoffman and Scribnerl removed single crystals of gallium solidifying in a gallium melt, while Zimmerman2 grew single crystals from the melt by the Kyropolous technique. In contrast, attempts at purifying gallium by zone refining have been less successful. ichards, reported that despite the passage of 40 zones through a gallium ingot, there still remained 5 to 70 ppm each of Cu, Fe, Ca, Mg, Si, Al, and Ag. Previously, Detwiler and Fox4 detected only one impurity, Pb, segregating in zone-refined ingots. These surprising results prompted an investigation of the factors controlling impurity segregation in gallium. Possible reasons for this were insufficient diffusion of impurities in the melt; recontamination of the melt by its oxide film which is not affected by the passage of the zone; reaction of gallium with the boat; sudden freezing of gallium following supercooling, especially since gallium easily supercools to and trapping of impurities at grain boundaries. Impurity segregation tests were carried out by directionally freezing gallium using the Bridgman rnethd, modified in that the molten gallium is lowered out of a furnace into a slush of dry ice and trichloroethylene, thus minimizing supercooling. Since the gallium is contained vertically, the oxide film is in contact only with the tail end of the melt. It was found that Teflon makes an excellent crucible for gallium since it is quite pure, non-reactive, translucent, flexible, machinable, and is not wet by gallium. The gallium crystals could be grown at various speeds, and the melt could be vigorously stirred by a Teflon rod moving through the gallium in a vertical reciprocating fashion. Single crystals could be grown by placing a solid Teflon plug at the bottom of the melt drilled out in such a way to cause the solidifying gallium to follow a winding path. Thus, even if many crystals are originally nucleated, only one grain will predominate. The grain structure of the gallium crystals was revealed by an etchant composed of equal volumes of HC1, HNO3 and HF, diluted with water to half strength. Emission spectrographic analyses were carried out on samples removed from the front and tail ends of the resulting gallium ingots. Typical results of this study are summarized in Table I. The rate of freezing in all three cases was about 1 in. per hr. It can be seen that even though stirring of the melt does help, it is even more important to grow a single crystal of Ga in order to obtain good segregation of impurities. The effect of crys-tallinity on the segregation of impurities was previously observed6 in the directional freezing of germanium; however, in this case, the effect was much less pronounced. This dependence of impurity segregation on the crystalline perfection of Ga may be related to its thermal conductivity which is the most anisotropic of all metals.7 The anisotropic thermal conductivity can cause the solid-liquid interface to be nonuniform, thus leading to trapping of impurities during freeing, and therefore reduced segregation. In conclusion, it is indicated that zone refining of gallium would be more successful if seeding and similar precautions are taken to insure single crystal growth. The authors are indebted to Mr. H. H. Whitaker for the spectrographic analyses and to Drs. B. Abeles and F. D. Rosi for helpful advice and encouragement throughout the course of this work. This research was supported by the Electronics Research Directorate, Air Research and Development Command, under Contract No. AF33(616)-5029. REFERENCES 'J. 1. IToffmon and B. T. Scribrer: I. Research h'atl. Bur. Standards, 1935, "01. 15, p. 205. 'W. Zirnmerman: Science, 1954, vol. 119, p. 41. %J. L. Richards: Nature, 1956, vol. 117, p. 182. 'D. P. Detwiler and W. M. Fox: I. Metals, 1955, "01. 7, p. 205. 5P. W. Bridgman, Proc. Am. ilcod. Sci., 1925, vul. 60, pp. 305,385,423. "S. L1. Christian: private c ommuni cation. 'K. W. Powell: roy. Sac., 1951, vol. 209, p. 525. 'W. G. Pfann: Zone Re fining, p. 20. John Wiley and Sons, Inc., New York, L058.

Jan 1, 1962