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By Charles H. Morgan

Jan 1, 1905

By Albert A. Mathews

OUTCROPS of gypsum rock near the present site of the city of Gland Rapids, Mich., were known to fur traders early in the nineteenth century. However, the deposits seemed without value and were not worked for some time. So far as cat1 be learned, Michigan gyp- sum was first used by a plasterer who settled in Grand Rapids in 1834 as a member of its fourteenth white family. In building a house for one of the early traders, be used some otnamental stucco mouldings manufactured from the local gypsum deposits for decorations in the gables and around some circular windows. The gypsum was broken out with a hammer, ground in an Indian corn mill, and burlled in a caulclron kettle,. After two attempts, the ornaments were successfully set, and remained on the house until it was destroyed by fire in 1850.

Jan 1, 1936

By Jesse O. Betterton, Y. E. Lebedeff

AS a matter of the most widespread interest to lead-refining metallurgists, the process of desilverizing lead originated by Parkes is the most fundamental step in lead refining. While this basic operation, in addition to effecting a practically complete recovery of gold and silver, is also a great purifying operation and a governor on the purity and uniformity of the final refined lead, it has the important deficiency that no bismuth is removed in the operation. The problem of finding a satisfactory, inexpensive method for removal of bismuth that would fit in with the basic desilverization step has been one of enticing interest for lead-refinery metallurgists for many years. Of late it has become one of imperative interest, and while many attempts and much progress have been made, it is probably fair to say that metallurgical progress thus far is only catching up with commercial requirements. The Pattinson process, an original competitor of the Parkes process for desilverization, has received much attention for its possibilities for bismuth removal. Bismuth concentrations in the Pattinson process fall far short of the silver concentrations and as a result too many operations are required and a crawl in grade in the kettle units is experienced which requires periodic correction. Altogether, it has proved too expensive a remedy, from the cost standpoint of both installation and operation. The Betts electrolytic process is a fully satisfactory remedy but its present status in the field of lead refining is more a matter of bismuth removal than preference as a refining system, except, of course, in instances particularly favorable to the basic requirements of the process. The Betts process, of course, is essentially different from the Parkes process, and very difficult to associate therewith to any economy except in minor ways. Accordingly, where economy dictates the Parkes process, and this is true of far the greater portion of the world's tonnage, the adoption of the Betts process primarily for bismuth removal is apt to prove an expensive remedy on account of its normally higher cost of operation, inelasticity of the equipment for variable tonnages, and high per ton cost of installation.

Jan 1, 1937

By W. R. Ingalls

THE bases of the work by the committee whereof I am chairman were (1) the abolition of extra-lateral rights and (2) the preservation of the maximum of the existing laws. The matter of extra-lateral rights had been under prolonged discussion among mining men and up to the time when our com-mittee began its work (in 1917) the expression of opinion in every way whereby it could be made known -and those ways were extensive-was only a little short of being unanimous that extralateral rights ought to be abolished. I have not observed important evidence indicating a change of opinion on the subject since 1917. ABOLITION OF DISCOVERY LOGICAL Now, when it be decided that extralateral rights ought to be abolished, there can not be merely a simple change to that effect, but it is found that consequential changes are necessary all the way through the existing laws. Abolition of extralateral rights implies abolition of discovery as a prerequisite to location, for otherwise there would be no legal means for locating claims on the dip of a vein. Quite apart from this consideration, abolition of discovery as a prerequisite to location is supported by other good reasons. Among these are the occurrence of orebodies with no exposure on the surface and which often are hidden at great depth. A prospector who has reason to suspect the occurrence of such an orebody must have legal means for the location of a claim within which to explore, and obviously he may. not be able to make any discovery on the surface sufficient to locate and hold legally such a claim under the terms of the law as it stands at present. As a matter of fact, discovery as a prerequisite to location was abolished by common consent many years ago, not only for the reasons that I have given here-inbefore but also for others. It is highly desirable to revise the mining law in this respect, so that it will conform to the conditions of practice and not require people to perjure themselves in making locations, even if it be for praiseworthy purposes.

Jan 6, 1922

EUGENE WESLEY SHAW,* Washington, D. C. (written discussion ?).-Studies of the probable future production of oil wells and fields-particularly those in the nature of the recent work by Lewis and Beal, having the object of increasing the percentage of recovery-rank, in both practical and theoretic value, very high, if indeed they do not outrank all other petroleum investigations except structural surveys. Even such surveys, although saving untold millions that might have been spent in prospecting unpromising territory, may have less ultimate value than generally supposed, for it may perhaps be argued that much if not most of the condemned territory will sooner or later be tested-some is already productive-and the most that can be rightly claimed is the recovery of cream first; also that the consumption of the richest portions first cannot be extenuated, as it might with some resources, on the ground that if the best is not taken now it will deteriorate.

Jan 5, 1918

By Lloyd R. Jackson

IN the past 15 years there has been a great deal of interest in the fundamentals of plastic flow and rupture in metals and a number of papers have presented substantial advances toward a fundamental insight into the mechanism of these two processes. This paper is an appraisal of the present position with respect to the following: I. The relative importance of shear and hydrostatic stresses in controlling the plastic flow of metals. 2. The relative importance of shear and hydrostatic stresses in determining the amount of flow before rupture in metals. 3. The use of generalid strains in determining the effect of plastic flow on the work-hardening of metals. FUNDAMENTALS INVOLVED IN PLASTIC FLOW In attempting to devise a quantitative description of plastic flow in metals, it has been customary to assume that metals are homogeneous and isotropic. The fact that neither of these assumptions is correct complicates the experimental appraisal of relations developed. Never- the less, as will be shown, metals are close enough to being isotropic and homogeneous so that considerable insight into the mechanism of plastic flow can be obtained. The assumptions of .isotropy and homogeneity allow both the elastic and plastic behavior of metals to be described in terms of 12 variables-six being stress variables, and six being strain variables. ) From this viewpoint, it should be possible to represent the stress-strain relations in the plastic range for metals by a surface in 12 dimensions. One boundary of this surface would be the surface of transition from elastic to plastic behavior; the other would be the surface of rupture. These two surfaces would be joined by the surface of plastic flow. The shape of this composite surface would depend on the test temperature and speed of straining. This paper is concerned only with results obtained at constant temperature and constant speed of straining. While such a representation is conceivable, the demonstration of such a surface would present almost insurmountable obstacles. The most fruitful simplification of this concept has been the recognition that the behavior of metals in the plastic region is primarily a result of shear stresses and strains. Based on this viewpoint, it is possible to utilize stress and strain invariants that are independent of hydrostatic components to define an effective stress and strain. In effect, this amounts to reducing the task of representing stresses and strains in 12 dimensions to one of representation in two dimensions. The two invariants (one for stresses . and one for strains) that have received most attention are the following: [ ]

Jan 1, 1946

By L. W. Holm

This study shows that in the presence of foam, gas and liquid flow separately through porous media representative of reservoir rock. These results were obtained by using tracer techniques to measure the flow of the gas and liquid comprising the foam. Foam does not flow through the porous medium as a body even when the liquid and gas are combined outside the system and injected as foam. Instead, the liquid and gas forming the foam separate as the foam films break and then re-form in the porous system. Liquid moves through the porous medium via the film network of the bubbles and gas moves progressively through the system by breaking and re-forming bubbles throughout the length of the flow path. The flow rates of the gas and liquid are a function of the number and strength of the films in the porous medium. There is no free flow of gas; i.e., no continuous gas phase. On the basis of these results, foam can be expected to improve a water flood or gas drive by decreasing the permeability of the reseruoir rock to a displacing liquid or gas. This improves the mobility ratio and thus the conformance of the flood. INTRODUCTION Foam is formed when gas and a solution of a surface active agent are injected into a porous medium either simultaneously or intermittently. During the past few years, several papers have been published on the subject of foam flow in Dorous media. Foam has been used successfully in the removal of capillary water blocks from producing formations.''2 The use of foam in gas storage reservoirs to reduce gas leaks and to increase storage capacity has been considered in recent years. Foam has also been investigated as an oil displacing agent,3-5 and as an agent to improve the mobility ratio in a waterflood.6-10 However, the mechanism by which the gas and liquid phases comprising the foam flow through a porous medium has nor been described adequately. Normally, when two immiscible phases (gas and liquid) flow concurrently through a porous medium, each phase follows separate paths or channels. At given saturations of the two phases, a certain number of channels are available to each phase, and as saturations change, the number and configuration of the channels available for each phase also change. The effective permeability of each phase is a function of the saturation of that phase only, and the flow of each phase can be described by Darcy's law. When foam is present, the effective permeability of the porous medium to each phase is greatly reduced compaced with permeabilities measured in the absence of foam.6,11-13 Based upon the observed flow of surfactant solutions and gas in capillaries, it has been concluded that the gas and liquid may flow separately or they may flow combined as foam. At least four mechanisms have been postulated to explain how fluids flow with foam present: 1. A large portion of the gas is trapped in the porous medium and a small fraction flows as free gas, following Darcy's law.9 2. The foam structure moves as a body; the rate of gas flow is the same as the rate of liquid flow. 6,13 3. Gas flows as a discontinuous phase by breaking and re-forming films. Liquid flows as a free phase.12 4. A portion of the liquid and gas move as a foam body while excess surfactant solution moves as a free phase.14 It also has been suggested that different flow mechanisms exist for high quality (dry) foams made from dilute surfactant solutions and for foams made from more concentrated solutions. Studies conducted on the flow of foam through capillaries have shown that a plug-type flow occurs and that foam flows as a body.6,15 Fried also has described the flow of foam through porous media as

Jan 1, 1969

By Clemens Jones

The difficulties attending the reduction of ferric sulphate in the determination of metallic iron by the method of Marguerite, are often serious, and affect time, patience and accuracy. They depend upon the condition and purity of the zinc used, the state of saturation of the solution, acidity, and temperature. D. J. Caruegie (Chem. News, lvii., No. 1481), says that ferric solutions are instantaneously reduced by the use of zinc-dust. But there are obvious objections to its employment in quantitative work. Dr.

Jan 1, 1889

By S. Acar, P. Somasundaran

The results obtained for the selective flocculation of natural ores do not usually agree with the corresponding properties of the constituent minerals when present alone. This is mainly due to the presence of dissolved mineral species which can interact in many ways with other components in the system and alter their behavior. In this paper, the effect of dissolved species on the flocculation and electrokinetic properties of sulfide minerals is discussed. Dissolved iron, copper, and nickel (Fe, Cu, and Ni) species are found to affect the properties of natural chalcopyrite and pentlandite in certain pH range. These effects are interpreted in terms of species adsorption leading to activation or depression of reagents, surface precipitation, and complexation of species

Jan 1, 1986

By AIME

D R. GILLSON, who was born in Evanston, Ill., in 1895, is another one of those geologists who received his early inspiration and foundation in his science from that great teacher at Northwestern University, the late Professor U. S. Grant, and then went on to give his time and interest to Institute affairs-like those other Northwestern men, Arthur Blair, Gilbert Cady, Charlie Behre, Evan Just, Ian Campbell, Clayton Ball, and many others. After serving in the Navy in the first World War as, of all things for a geologist, a commissary officer on a transport, he went on to MIT and took his doctor's degree under Waldemar Lindgren in 1923. He even assisted in mineralogy at Harvard and thus had training under another great teacher, Charles Palache. He taught mineralogy and petrography at MIT from 1923 to 1928. After several summers of field work as an assistant in the U. S. Geological Survey, Dr. Gillson joined the staff of the du Pont company.

Jan 1, 1947

By Richard H. Sprute, Dennis J. Kelsh

Slow-settling, fine-grained suspensions can often be dewatered and densified by applying direct current between buried electrodes. Although water removal rates and power expenditures depend on physical and chemical properties of the treated slurries, metal mine tailings from Idaho, Colorado, and Mexico have responded well in laboratory testing, as have 29 samples of ultrafine coal waste from mines in nine states. This Bureau of Mines report reviews field tests at two Idaho metal mines and describes the recent installation at the Henderson molybdenum mine near Empire, Colorado, and the treatment of coal sludge at a Clinchfield Coal Co. preparation plant near Dante, Virginia.

Jan 1, 1980

By A. C. Wallace

THE development of the natural resources of any district of any magnitude, inevitably gives rise to many problems off title, usually due to the greatly enhanced value of the land. The development of the mining industry in the Quapaw Agency has been no exception to this general rule. Our problems, how-ever, have not been many or particularly serious. The Quapaws were allotted and patents issued by the United States Government in 1895. These patents contained a restriction against alienation for a pe-riod of twenty-five years. The effect of the restric-tion was to prevent the Indian from selling, leasing, or in any way encumbering his land. The Govern-ment, in a paternalistic spirit, sought to teach the Indian thrift and industry and to insure him a place of residence. This is evidenced by the first Leasing Act passed by Congress, which permitted only incom-petents and those physically disabled to lease their land for either agricultural or mining purposes. The able-bodied Indian was denied the right to lease. It soon became apparent to the Government, how-ever, that this was a mistaken policy, and in 1897 a General Leasing Act was passed by Congress and it was under this act that the mining industry in the Quapaw Agency was developed. The act, reads as follows: "That the allottees of land within the limits of the Qua- paw Agency, Indian Territory, are hereby authorized to lease their lands, or any part thereof, for a term not ex-ceeding three years, for farming or grazing purposes, or ten years for mining or business purposes. And said al-lottees and their lessees and tenants shall have the right to employ such assistants, laborers, and help from time to time as they may deem necessary: Provided, That when-ever it shall be made to appear to the Secretary of the Interior that, by reason of age or disability, any such allottee cannot improve or manage his allotment properly and with benefit to himself, the same may be leased, in the discretion of the Secretary, upon such terms and conditions as shall be prescribed by him. All acts and parts of acts inconsistent with this are hereby repealed." It was the interpretation of this Act that gave rise to our first serious problems. It will be noted that the Act says that "allottees of land" within the limits of the Quapaw Agency are authorized to lease their land. Thus, the first question was presented by the use of the term "allottee," and the question was as to whether or not Congress intended to limit the Quapaw Indian to the leasing of his own allotment or did Congress mean that the term "allottee" was synonym-ous with "Indian" and intend to give the Indian a right to lease both his allotment and his inherited land and was an Indian without an allotment an "allottee" even though he was a member of the Qua-paw tribe and the owner of the Quapaw land by in-heritance, and not being an allottee, could he lease his inherited Quapaw land under the authority granted in this Act?

Jan 5, 1928

By A. E. Bellis

THE CHAIRMAN (ALBERT SAUVEUR, Cambridge, Mass.).-Any information likely to throw light on the constitution and proper treatment of high-speed steel in order to obtain maximum results, should surely he welcomed. All users of high-speed steel, I believe, will agree with the authors that, in order to obtain satisfactory results, it is not sufficient to heat all brands of high-speed steel to one and the same temperature; apparently very slight differences of chemical composition seem to call for marked differences in temperature. I think that all of us agree that a properly treated piece of high-speed steel should have a fine austenitic or polyhedral structure and that an appreciable quantity of free carbide may be present in the case of very high tungsten steels. What we seem to lack is a satisfactory method, quick and reliable, of ascertaining when the proper structure has been obtained. I think Mr. Bellis' paper is a step in the right direction. To the untrained eye, however, it is not an easy matter to select from some of his photomicrographs the one representing the best structure; for instance, in the case of steel A, we wonder why temperatures of 2,250 and 2,300 do not yield the same results, seeing that both structures are apparently alike, and the same might apply to some of the other samples. I have no doubt, however, that the experienced observer is capable of detecting structural differences that are not made plain here and by which he is able to select the proper quenching temperature. COLIN G. FINK, East Orange, N. J.-On page 68 the authors say that the use of a barium chloride bath to eliminate this difficulty has the disadvantage that the surface of the tool becomes decarbonized." I would like to ask whether they actually found that the surface was decarbonized, or whether they base this conclusion on softening alone? A. E. BELLIS, Springfield, Mass.-No, we have never demonstrated that it was a decarbonization, it is just the softening of the steel. The addition of ferrocyanide to the ferrochloride bath has been suggested. I think that is not altogether satisfactory, because the ferrocyanide bath changes composition very rapidly at these high temperatures, and it would be just a question of luck whether or not it had too much or too little ferrocyanide in the bath giving equilibrium with the carbon content.

Jan 4, 1917

By H. H. Pentz

This paper gives the derivation of a practical formula for the calculation of slopes in seismic reflection prospecting. The derived formula is an approximation and can be used where the slope of the reflecting horizon is less than 250 ft. per 1000 and the depth to the reflecting horizon is greater than 2500 ft. The slope of sediments in oil regions is generally considerably less than 250 ft. per 1000. This is particularly true of the Gulf Coast, with the exception of the salt domes, which usually have the sediments at a greater slope than 260 ft. per 1000. Derivation In Fig. 1, o represents the image of the shot point a. Then the length of the path acb is equal to ob and ae'd is equal to od. In the triangle aob, p is equal to ob, x is equal to , and c is equal to ao. The angle u is the apparent dip of the reflecting horizon. Angle oab is equal to (90" - u). The quantity m is the slope of a line tangent to the curve, defined by equation 1, at the point (p, x). The quantity m' is the slope of the line tangent to the curve at the point (p', 2').

Jan 1, 1940

By H. H. Pentz

This paper gives the derivation of a practical formula for the calculation of slopes in seismic reflection prospecting. The derived formula is an approximation and can be used where the slope of the reflecting horizon is less than 250 ft. per 1000 and the depth to the reflecting horizon is greater than 2500 ft. The slope of sediments in oil regions is generally considerably less than 250 ft. per 1000. This is particularly true of the Gulf Coast, with the exception of the salt domes, which usually have the sediments at a greater slope than 260 ft. per 1000. Derivation In Fig. 1, o represents the image of the shot point a. Then the length of the path acb is equal to ob and ae'd is equal to od. In the triangle aob, p is equal to ob, x is equal to , and c is equal to ao. The angle u is the apparent dip of the reflecting horizon. Angle oab is equal to (90" - u). The quantity m is the slope of a line tangent to the curve, defined by equation 1, at the point (p, x). The quantity m' is the slope of the line tangent to the curve at the point (p', 2').

Jan 1, 1940

By A. Beeby Thompson

FOR more than 2500 years, natural gas issues in the Surakhany district of the Apsheron peninsula were the object of pilgrimages by fire worshippers and Hindoos from Burma and India. Even as late as 1890, Hindoo priests conducted ceremonies in a temple at Surakhany, which probably replaced a more ancient one; but later, the visits of the pilgrims were prohibited in order to check the spread of Asiatic diseases in that region. For centuries, limited supplies of oil have been abstracted from shallow excavations in the Caspian oil belt and dispatched into the interior of Asia and elsewhere for medicinal and industrial purposes. Statistics show a yield of 37,400 bbl. in 1863, but only since 1869 has there been serious development; in that year the yield was 203,000 bbl. At that time, hand digging was supplanted by drilling, and the enormous wells that resulted from tapping sources hitherto beyond the reach of operators completely demoralized the industry for a time, owing to inadequate outlets for the products. The early activities in this area were greatly hindered by annoying taxation, monopolies, imperial land grants, etc., but when these were revoked or adjusted, in 1877, the industry sprang into prominence and, between 1898 and 1901, the Baku fields produced practically one-half of the world's supply of oil. Within a few miles of Baku lie the two richest oil fields in the world; viz., the Balakhany-Saboontchy-Romany and the Bibi-Eibat, the latter constituting almost a suburb of the city. For many years the gasoline obtained in the refineries of the Baku area was burned in pits, being considered an undesirable product, and until 1870 the residue also was destroyed, its value as a fuel not being recognized. Kerosene was the main product sought by the refiners. It was shipped across the Caspian Sea and up the Volga to the industrial centers of Russia. Only on the completion of the Baku-Batoum railway did the Baku oil fields secure

Jan 8, 1920

By E. T. Turkdogan, P. Grieveson

It is shown experimentally that, by making use of the coupled S-O reaction in ionic melts, it is possible to transfer slclJur or oxygen from a lozv to a high chemical potential through an ionic nzenzbrane. This uphill transfer of sulfur is accompanied by a counter downhill transfer of oxygen and vice versa. The Materials balance shows that the amoulits of sul -fur and oxygen lost or gained by one system are the same as those gained or lost by the other systenz — the two systejns being separated by an iofzic membmne. The systems used in these experi?nents were solid Mn-MnS-Mno and liquid Fe-S-0. Sufficient results were obtained Lo study the kinetics of the transfer and the indications are that the counter diffusion of sulfide and oxide iojzs in the membrane is the rate controlling process. WHEN an ionic oxide-melt reacts with an atmosphere containing sulfur and oxygen-bear ing gases the following reaction occurs: 1/2 S2 (gas) +O2- (melt) = S2- (melt) + 1/2 0, (gas) [1] Under the restrictions that i) electric conductance in the melt is purely ionic and ii) each constituent element in the melt does not change valence, the solution of an atom of sulfur in the melt will result in the evolution of an atom of oxygen, so that the electric neutrality is maintained. For a given temperature and melt composition, the equilibrium concentration of sulfur in the melt is determined by the ratio, po2 /ps2 , in the gas phase and not by the individual partial pressures of oxygen and sulfur. This has been demonstrated by a number of investigators, for example by Richardson and withers', Fincham and Richardson,la by St Pierre and Chipman,' and by Turkdogan and Darken.3 In his Howe Memorial Lecture for 1961, Darken discussed the possibility of uphill pumping of sulfur through an ionic membrane at the expense of oxygen. TO test the validity of this concept associated with coupled reactions, experiments were carried out in the following manner. A presintered mixture of Mn-MnS-MnO and prefused mixture of Fe-S-0, contained in platinum and iridium crucibles, respectively, and separated by a thin layer of soda-glass (to act as an ionic membrane), were placed side by side in an evacuated silica capsule and sealed. This was then kept at 1400°K for a required time to allow Reaction [11 to occur via the ionic membrane. When partial equilibrium is reached, the ratios Po2 /pS2, for systems on either side of the membrane, are equal and the flux of sulfur and oxygen through the membrane becomes zero, although the individual partial pressures po2 andp,, in these two systems may differ considerably.

Jan 1, 1962

By T. Sterry Hunt

Jan 1, 1891

By W. M. Peirce

WITH the supply of zinc, like that of most other nonferrous metals, inadequate to meet the demand, efforts to increase domestic ore supplies and production capacity have been of primary interest. No major sources of new ore have been disclosed during the year but improvements have been reported in facilities for mining and concentrating ores from existing mines. The American Zinc, Lead and Smelting Co. has announced its intention of erecting a new mill in the Ouray district of Colorado. The Consolidated Mining and Smelting Co. of Canada is reported to be planning improvements costing $3,000,000 to its Sullivan mine and concentrator at Kimberley, B.C., where the sink-float process is to be used for preliminary ore treatment. In the reduction field, the St. Joseph

Jan 1, 1947

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