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By W. E. Horst

Flotation feed was hell constant for batch laboratory tests and continuous pilot and commercial plant tests on a spodumene ore to determine the relation.ship between flotation behavior and the size and type of flotation machine. Results. showed that additional retention time would be needed in the plant flotation circuit to duplicate laboratory or pilot plant performance when operating Dariables of the. plant flotation machines remained unchanged. During the past few years of operation at Kings Mountain, N. C., full-scale flotation has generally yielded poorer metallurgical results than those obtained in the laboratory or pilot plant. After 2 min in each size of Denver flotation machine in the spodumene rougher circuit, pilot recovery (41.7 pct) was almost three times that of the plant (13.6 pct) and about twice that of the laboratory (21.0 pct). Pilot and commercial plant data are based on continuous operation, and laboratory results on batch testing of rougher performance. The ore is a pegmatite containing spodumene, feldspar, quartz, mica, and amphibolite. Data were accumulated to evaluate the scale-up relationships between laboratory, pilot plant, and plant flotation cells. Flotation rate constants and dimensional analysis were used to define the relationship existing between flotation behavior and scale of operation. Measuring Flotation Rates: Efficiency of the rougher stage was measured by flotation rate, defined as the recovery that can be attained within a given time." • The problem of measuring flotation rates has been studied by many investigators, whose methods have varied. Published studies an flotation kinetics have been summarized recently by Gaudin.l When comparing flotation rates, it is more satisfactory to compare straight line relationships between recovery and flotation time than exponential curves resulting from plotting cumulative recovery vs cumulative flotation time. To convert the exponential curves into straight line relationships, rate equations were applied similar to those used in chemical kinetics to study the velocity of chemical reactions. Two rate equations have been used in this investigation to measure efficiency of the various cells: 1.5 order Rate Equation dR/dt=k (A-R)1.0 [Eq.1] Second Order Rate Equation dR ---- - K(A - R)2 [Eq. 2] dt Upon integration Eq. 1 becomes 1/(A-R)1/2=k/2 t+1/A1/2 [Eq. 3] and Eq 2 becomes: or fEq. 4] t/R=1/A2K+t/A [Eq. 4] where R = cumulative recovery [percent recovery of total value (spodumene) in flotation feed]. A = initial concentration, pct (100 pct of mineral to be separated). t = flotation time (minutes). k = flotation rate constant for 1.5 order rate equation [units: 1/(percent) 0.5 (min)1. K = flotation rate constant for second order rate equation [units: 1/(percent) (min) 1.

Jan 1, 1959

By R. W. Nelson

Methods for determining permeability presented by W. D. Kruger3 in a paper entitled "Determining Areal Permeability Distribution by Calculation" have considerable merit. They can be expected to contribute significantly to analysis of flow in heterogeneous systems. Some rather subtle yet important conditions must be met, however, to assure that the computed permeabilities are correct. The conditions which insure a unique permeability distribution may have been overlooked in the method as proposed and presented in the subject paper. The subtlety of the special requirements may permit good agreement between computed and measured pressures in the reservoir; but the computed permeability may still be in error. The general theory and discussion of the requirements for a unique determination of the permeability distribution are presented elsewhere in more detail.7'8 Accordingly, only major features will be presented here in the notation of Kruger. GENERAL DESCRIPTION OF REQUIREMENTS A brief mention of the route to be followed in showing the special requirements may be helpful. The equation to be solved is a quasilinear, first-order, partial differential equation in the unknown permeability. This equation can be solved through an extension of Lagrange's method by reduction to a system of subsidiary ordinary differential equations. Through consideration of the identity of one of the Lagrange subsidiary differential equations with the stream function, a special interrelationship can be shown. The interrelationship has special significance with respect to the boundary condition. If the boundary function satisfies part of the subsidiary differential equation, no unique solution for the permeability distribution exists. In the physical problem this requirement for uniqueness indicates that the permeability measurements used as a boundary condition can not be along a stream tube. The boundary condition must be along a line, or series of lines, which completely traverse the region and pass through every stream tube.

By AIME AIME

SOME 65 members of the Institute, including most of the Local Section delegates and several Directors and officers, were on hand for the Annual Business Meeting of the Institute held in the Engineering Societies Building on Monday, Feb. 21, at 4:30 p.m., immediately following the second session of the Local Section Delegates Conference. President Mathewson presided. The meeting was largely taken up with the presentation of committee re- ports, discussion of which was invited. F. E. Wormser presented the report of the Admissions Committee ; Philip Kraft, Papers and Publications Com-

Jan 1, 1944

By Leonard A. Wood, A. G. Winslow

Subsidence has occurred in several areas of the upper Gulf Coast region of Texas, although in most cases this is not evident without precise instrumental leveling. As referred to in this report, the region com- prises about 7200 sq miles of the Gulf Coastal Plain and includes all or parts of the following counties: Harris, Fort Bend, Waller, Brazoria, Galveston, Liberty, Chambers, Orange, and Jefferson (Fig. 1 ). Topographic relief is low, ranging from sea level at the Gulf of Mexico to 300 ft or more in northwestern Harris County.

Jan 10, 1959

By A. G. Suydam

Ancient as is the art of producing copper, so ancient is one of its eternal problems: refractories. Looking backward, in the light of present knowledge, clouded though it be, one cannot avoid a sense of profound respect for the patience, acumen and courage of those who have wrought so successfully despite difficulties, a more accurate understanding of which seems merely to accentuate. The problem of refractories arises from the necessity for constructing containers in which to bring natural ores into thermal solution in order to effect reduction and separation of the valuable metal content and free it of undesirable contamination while producing a waste slag. The very forces known to produce thermal solution of sufficient liquidity are necessarily destructive of exposed refractory linings in proportions varying inversely with thermal conductivity, directly with the porosity and ease of fluxing of the refractories used, and directly with the temperatures employed. Beyond this, mechanical forces are set up within the refractory lining incident to rapid heating or cooling, shrinkage at high temperatures, and unequal or excessive loading, that frequently pass the elastic limit, causing spalling or distortion. The effects of these forces are often accentuated by the necessity of providing at the same time as hot a bath and as cool a container as are consistent with fuel economy. Evolution in the Use of Refractories Clay Brick.—Fireclay and clay refractories had to yield wherever they were in contact with slags rich in basic oxides, first because of the combining power of those oxides with free silica and secondly because of the tendency of alumina to form either aluminates or alumina-silicates of varying complexity. Of no less importance, the incipient fusion point was low as compared with good clay brick of today, while the brick lacked strength at high temperatures. Expansion was slight, therefore it was difficult to make and maintain tight walls, roof, or bottom. However, the spalling tendency was low because of some of these properties and clay brick have retained their place in roasting furnaces, boiler furnace linings, and in the upper walls of some of the reverberatory types such as some refining, anode and wire-bar furnaces. They have served often and most efficiently for hot patching.

Jan 1, 1934

By T. F. Witherbee

ON the 22d of November, „1879, white iron unexpectedly appeared while working the Cedar Point Furnace, Port Henry, N Y., on the following burden, calculated to turn out mill and foundry iron: Anthracite coal, - 3000 pounds. Connellsville coke, - 1500 pounds. Total, - 4500 pounds. Old Bed ore, - 3750 pounds. New Bed fine ore, - 2000 pounds. New Bed chunk ore, - 1000 pounds. Kearnev hematite ore, - 750 pounds. Total, - 7500 pounds. Magnesian limestone, - 1865 pounds. Common limestone, - 885 pounds. Total, - 2500 pounds. The production per week since making mill iron-from September 1st, 1879, to date, seven weeks-was 412 gross tons. Ore was not immediately taken off, as nothing serious was looked for. The iron for the next week graded from No. 4 to white, and in. six days the make was 274 1/2 tons. At 10 P.M., Friday, the 28th, a slip of-..4 feet occurred, and on Saturday, at 5 A.M., another of 3 feet on the south side and. 7- feet on the north side took place. At this time it was found that the south side had been hanging for over a week--a fact which had not been reported. Throwing off the wind, to produce slips. and reduce pressure, had been tried with no effect. The stock, as seen through the tuyeres, seemed to consist almost entirely of coal, with just enough infusible cinder to cement it into a mass through which the blast could not be forced. At 3.50 A.M., Sunday, the 30th, the first cinder seen in seventeen hours came into tuyeres Nos. 1, 2, 3, and 6, At 9.30 A.M. No. 3 was taken out to see if the stock

Jan 1, 1881

By Fred A. Hale

Owing to the large area included in the Yellow Pine mining district, and the varied nature of its mineral deposits, a detailed geological description of the district could be covered only in an extensive monograph. This paper is intended as a description of the most prominent geologic features only with special reference to those of economic importance. The first mention of the district was in 1903 by J. E. Spurr, who briefly describes the structural geology of the Spring Mountain range. In 1906, H. F. Bain2 briefly described the Potosi mine. James J. Hillla of the United States Geological Survey, visited the district for a brief period in 1912, the result of which is an excellent reconnaissance report, covering the district in some detail but necessarily with brevity. Since that time, articles covering special features of the district have appeared in the technical press, including some by the writer, and a notable description of the Boss mine, by Adolph Knopf,4 appeared in 1915. Development of the district during the past few years has progressed so rapidly and with so many notable discoveries, particularly with reference to the rare metals, that a further description at this time may prove of interest. The writer's acquaintance with the district is based on 7 years' continuous residence in the vicinity, beginning with the spring of 1910. A. Location and Topography The Yellow Pine mining district is situated in the southwestern portion of Clark County, Nevada, about 300 miles northeast of Los Angeles, along the line of the Los Angeles & Salt Lake Railroad. The district extends from Mt. Olcott on the north to the California line on the south,

Jan 1, 1918

By Erwin H. E. Gaertner

The brown-coal opencast mines in Germany's Rhineland have to cope with several problems. Predominant are densely populated areas with highly productive farmland, many railroads, highways, and rivers, as well as towns and farm settlements which have to be removed before or during the lifetime of a mine. Also the ground- water table has to be lowered to keep the deep opencast mines dry and stable. These problems urged a development towards deep opencast mines with powerful machines; the large material movement and the high coal production are the basis for the economic success in working the Rhenish brown-coal deposits. Up to now, bucket wheel excavators with a daily capacity of 100,000 m3 (130,000 cu yd) are in operation. Machines of twice this capacity are under construction. Corresponding to the excavators development, the stackers' capacity has to be increased too. The new stackers will reach a daily capacity of 240,000 m3 (310,000 cu yd). The haulage in the mine is performed by conveyor belt systems, which are arranged in such a manner that the belt lines meet at a belt switching point. Here the incoming lines may be connected to the outgoing ones so as to direct the material flow to the desired receiving stations. At the moment there are conveyor belts in operation with a width of 2.2 m (7.2 ft); the new belts will have a layout for 37,000 t/h (40,770 stph), the width of which amounts to 3.0 m (9.8 ft). All belts and driving stations on benches are shiftable.

Jan 1, 1976

By I. Cornet

With the greatly expanding use of magnesium during the war, it appeared necessary to the War Metallurgy Committee that the notch sensitivity of magnesium alloy extrusions be further investigated and the influence of various factors upon notch sensitivity be noted. Accordingly, the National Defense Research Committee of the Office of Scientific Research and Development placed a research contract with the University of California, supervised by the War Metallurgy Committee. The work discussed herein was done under "Restricted" Project NRC-21, reported in Dec. 1943~; it has been released for publica-tion by the O.S.R.D. Scope of the Investigation The notch sensitivity of various magnesium alloy extrusions was determined under axial tension, and also under several conditions of nonaxial tension. Hardness, grain size and other metallographic features were observed; stress-strain data were obtained, and the chemical compositions of the alloys were determined, in order to correlate these quantities with thc notch sensitivity. Notch sensitivity under axial tensile load was determined for a few specimens which had been cold worked to various degrees by tensile prestraining. Magnesium alloy extrusions studied included Dowmetal 0, X, J, and A(. For comparison, extrusions of aluminum alloy 24s-T, cast bars of aluminum alloy 122-T2, and cast bars of magnesium alloy C were also tested. The specified chemical composition of these alloys is given in Table I. All bars tested were within specification limits of composition. Investigation of thc tensile notch sensitivity of various magnesium alloy extrusions, under conditions of axial and eccentric load, showed little or no correlation with stress-strain or other conventional data. Since the many uncontrolled variables present might mask significant relationships, one alloy was selected for intensive study. Magnesium 0 alloy extrusions were subjected to experimental heat treatments, and the ,Changing hardness, tensile strength, microstructure, and notch sensitivity observed. Experimental Techniques and Procedures Tensile Testing Bars used for axial loading were machined with % in.- and with 34-in. minimum diam1 and included specimens with 60" V notches (Fig I and 2). Each V-notched specimen was roughed out carefully and then finished with a honed tool. These Y-notched bars were sampled frequently, sectioned, polished, and examined at 500 X magnification to control

Jan 1, 1949

By Strathmore R. B. Cooke

On the basis of experiments conducted on quartz using a bubble pick-up method, it was shown in an earlier paper1 that this mineral will preferentially adsorb hydrogen, calcium, or sodium ions, depending on the relative concentrations of those ions in the solution in which the quartz is immersed. For quartz particles ranging in size from 0.2 to 1 mm, it was demonstrated that the concentration of calcium in solution (assumed present as ions) necessary to completely activate quartz for flotation is given by the expression: Ca++ = [H+] X 106 + [Na+] X 10-3 In this expression, ionic concentrations are in mols per liter. It was further shown that the pick-up method is apparently more sensitive to changes in reagent concentration than the standard captive-bubble method, and that induction times are apparently much reduced. Since completing these earlier tests, a new type of cell has been constructed; this is shown in Fig 1 and 2. In Fig 1, A is a ground joint, B is a central tube reaching to within a few millimeters of the bottom of the cell, and C is a stopper which may be removed for reagent addition, and serves the further purpose of excluding carbon dioxide from the air during the test. The entire cell is constructed of Pyrex glass, and does not give the trouble experienced with the earlier cell, in which activating ions were released from the glass at high pH values. The only critical factor in the construction of the cell is the clearance between the central tube and the bottom of the cell. This clearance should be sufficiently small that the bubble can be pressed directly on the mineral grains lying on the bottom of the cell. In the pick-up tests to be described in this paper, the reagents used were all of C. P. grade, except the sodium oleate, which was Merck's "neutral powder." The quartz employed was water-clear vein quartz, sized on screens, cleaned with both hydrochloric acid and sodium hydroxide, and given a thorough final washing with distilled water. Experimental procedures were the same as described in the earlier paper. EFFECT OF SIZE OF QUARTZ ON PICK-UP To ascertain the effect of particle size on the adsorption of calcium ions, the quartz was sized from minus 14 plus 20 mesh through the intervening screen sizes to minus 270 mesh plus 400 mesh. Each size was thoroughly cleaned, and then tested in the cell at different calcium chloride and sodium hydroxide concentrations, and at a constant sodium oleate concentration of 20 mg per liter. All particles, within the size range given, exhibited complete pick-up within the curve expressed by the equation above. This presumably means, when the conditions imposed by the equation are satisfied, that this maximum is independent of particle size. However, it was found that the range through which partial particle pick-up occurred progressively broadened as particle size decreased. This is shown in Fig 3, in which curves B, C, and D show the limits at which pick-up just commences (as the pH is increased) for particles of minus 14 plus 28 mesh, minus 65 plus 100 mesh, and minus 270 plus 400 mesh size, respectively. These results indicate that for satisfactory activation, at any given pH, a lower calcium ion concentration is required for fine particles than for coarse particles. EFFECT OF HIGH ALKALINITY ON PICK-UP At calcium concentrations of between 1 and 10 mg per liter, and at high alka-linities, it was noticed that pick-up ceased as soon as calcium hydroxide commenced to precipitate. This effect was investigated at other calcium concentrations, with the same results. Solutions of calcium chloride, containing 105, 104, l03, and l02 mg of calcium per liter were made alkaline with sodium hydroxide until calcium hydroxide just started to precipitate, according to the following equation: CaCl² + NaOH -+ Ca(OH)2 + 2NaCl The beginning of precipitation was taken as that point at which either a faint opalescence appeared in the solution, or a Tyndall cone became ap-

Jan 1, 1950

By Harold B. Treweek

The development of full scale flotation circuits based on laboratory and/or pilot plant data is discussed. Auxilliary operations, equipment and layout essential for trouble-free start-up and operation are noted. The selection of flotation cell size is discussed as it affects plant capital and operation costs.

Jan 1, 1978

By J. W. Faust, H. F. John

Generalized conditions for rod or ribbon growth by the twin plane re-entrant edge mechanism are given. It was shown that this mechanism can result in growth of twinned platelets from dilute metal solutions. The platelrts 01 the fee metals are faceted by (111) planes and contain two or more twin planes. Microsegregation traces were revealed in silver grown from a thallium solution. VOGEL has already set down conditions for dendritic growth;1 however, this was the normal single-crystal dendritic growth experienced during solidification. In this work it is desired to set down the crystallographic conditions that will lead to rod or ribbon growth with smooth facets. These are as follows. a) The growth must be crystallographically limited (i.e., faceted growth). b) In order to have directed growth, some mechanism must allow easier nucleation than two-dimensional nucleation. That mechanism is afforded by the re-entrant edges at twin planes.213 Thus there must be twin planes present in the rods or ribbons. c) The growth direction must lie in the twin plane. If not, the twin plane will grow to the face or side of the ribbon and the site of easy nucleation will be lost. d) The growth direction must be parallel to at least one plane of the faceting planes, and no set of the faceting planes can be perpendicular to the growth direction. A corollary to these conditions involves the number of twin planes necessary to maintain the indestructible re-entrant edge. The number depends on the crystal structure of the material. An analysis of the data available shows that a material whose faceting planes form an open figure requires at least one twin plane while materials whose faceting planes form a closed figure require at least two twin planes in order to form the indestructible re-entrant edges for extended growth. The conditions and an assessment of the possibility of rod or ribbon growth are given in Table I for several crystal systems. As can be seen the fee, diamond and zinc blende, or-thorhombic, rhombohedral, and one form of the hexagonal lattice systems can yield this type of growth, but not the bcc metals nor the hexagonal

Jan 1, 1965

PAUL. D. MERICA, Bayonne, N. J. (written discussion*)..-The mode of intercrystalline oxidation which the authors" have so well observed and described is characteristic of nickel that has been exposed' to: the action of an oxidizing atmosphere at higher temperatures, such as, those at which; it is annealed or heated for rolling or forging. Oxidation under such conditions proceeds inward from the surface along the, crystal boundaries' producing a net-work, probably of oxide; which causes a very brittle condition of this surface material. This, in turn, generally results in surface cracking and checking during further, rolling and a defective sheet or other product is produced. An example of this is shown in Fig. 2, which shows the surface, of a badly surface-cracked sheet of nickel produced by incorrect heating con-ditions. A cross-section of this sheet etched with nitric acid is shown in Fig. 1, which reveals the intercrystalline oxidation network adjacent to both surfaces.These layers are so brittle that it is not possible to deform them by rolling without severe cracking along these lines or, planes of weakness. The best, and possibly only, remedy for this condition lies in its prevention by the maintenance of a neutral soft flame for heating and annealing nickel during the entire course of its manufacture. I should like to suggest that, those making microscopic investigations of nickel and nickel-rich alloys try the use of acetic-acid .solutions of nitric acid for etching these metals rather than aqueous solutions, of nitric acid. I have found that a solution containing 50 per cent. nitric acid, from 25-45 -per. cent. acetic acid, and from 25-5 per cent. water gives excellent results with. Wrought and cast nickel and Morsel metal and superior results to those obtained with nitric acid, alone. The acetic. acid seems to inhibit the passivity that nickel often assumes toward nitric acid and much more uniform etching may, be obtained. The proportions of nitric and acetic, acid may be varied somewhat from those given without mate-rially altering the quality of the etching, although without any distinct improvement in it.

Jan 12, 1919

By J. D. Milburn, H. J. Hill

In quantitative interpretation of electrical logs the presence of clay minerals introduces an additional variable which further complicates an already complex problern. Although recognizing the difficulties introduced as a result of the heterogeneity of natural sediments and despite the present incomplete state of knowledge regarding electrochemical behavior of shales, dissemirzated clay minerals and concentrated electrolytes, it was felt that useful empirical correlations might be obtained from experimental investigation. Six typical sandstone formations, having a wide variety of petrophysical properties, were selected for the study. Approximately 45 samples from each formation were selected to satisfactorily represent the range of pore size distribution within the particular formation, As a matter of general interest, four limestone formations were also included in the investigation. Previously proposed equations relating to resistivity, SP and interrelationship of the two phenomena have, where possible, been tested with data obtained in this investigation. These equations do not satisfactorily describe experimental behavior of samples through all degrees of shaliness or throughout the range of brine solution resistivities normally encountered in logging practice. An empirical equation has been developed which quantitatively relates formation resistivity factor to satirrnting solution resistivity, porosity, and "effective clay content." This relation is indicated to be uniformly applicable to clean or shaly reservoir rocks. It is shown that both the SP and resistivity phenomena of shaly samples are related to the sample cation exchange capacity per unit pore volume. The independent chemical determination of this parameter is thus a means of determining the "effective clay content" of samples. Some implications regarding theory and electric log interpretation of shaly sands are discussed. INTRODUCTION The use of electrical resistivity logs as a means for estimating formation porosity is based upon the original work of Archie1. It was shown by empirical methods that the resistivity of a rock, when 100 per cent saturated with brine solution, could be related to rock porosity through the equation, F = Ro/ RW = f-m.......(1) where F, the formation resistivity factor, is defined as the ratio of the resistivity of the 100 per cent water saturated rock, Ro, to the saturating solution resistivity, Rw; f is the ratio of pore volume to bulk volume; and m is the slope of the average line when the data are plotted on log-log paper. This relation was established for relatively shale-free formations containing water having high salt concentrations, and under these conditions F may be considered constant for a given rock sample. Applications of Eq. 1 to interpretation of logs of shale-free formations has been quite successful when satisfactory formation water resistivity data could be obtained. The most readily available means of estimating formation water resistivity is the self-potential log. Conventional methods of SP log interpretation involve correct.

Jan 1, 1957

Mining Methods GERALD F. SHERMAN, Chairman JOHN A. CHURCH, Vice-chaiman CHARLES W. WRIGHT, Secretary Alluvial Mining CLINTON BERNARD CHARLES JANIN H.R. NORSWORTHY Open-cut Mining Iron MAX H. BARBER J. A. MACKILLICAN Copper MICHAEL CURLEY R.B. TEMPEST Underground Mining Iron C. H. BAXTER TENNEY C. DESOLLAR

Jan 1, 1934

By W. R. Ingalls

ThE following chronology presents the history of lead-mining in the United States in a brief form and is a useful reference in connection with the statistics of production: 1621.. Lead was mined and smelted near Falling Creek, Va., to supply the local demand for bullets and shot. This was the first mining and .smelting of lead in what is now the United States. 1632. In a report made on the minerals of New England, lead-ore is mentioned. (Bishop, I., 470.) 1650. Supposed beginning of mining by Jesuits in Pima county, Ariz. 1651. Grant of lead-mine at Middletown, Conn., to Gov. John Winthrop. 1682. Lead-ore supposed to have been discovered in Wisconsin by Nicholas Perrot. (K. D. Irving, Mineral Resources of Wisconsin, Trans., viii., 498.) 1700 Discovery of lead in Missouri by Penicaut, one of Le Sueur's party. Tile same expedition discovered lead near the southern boundary of Wisconsin in August of the same year. 1712. Grant by Louis XIV. of the Crozat patents, with special privileges respecting the discovery and operation of mines in the then territory of Louisiana. Little or no mining was done under this patent until about 1720. 1717. Transfer of Crozat patents to the Mississippi Co., promoted by John Law, which prepared for active mining. 1719. First attempt to mine and smelt lead in Missouri, made by Sieur de Lochon, in behalf of the Mississippi Co., near Meramec river. Results unsuccessful.

Jan 1, 1908

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 G. G. Hancock, H. H. Johnson

Hydrogen gas at atmospheric pressure is shown to cause substantial embrittlement in a martettsitic high-stretzgth steel. Subcritical crack growth is observed at very lom stresses and with high growth rates. It is suggested that an adsorbed layer of hydrogen atoms at the crack-tip surface provides the damaging hydrogen. Oxygen in small quantity, as little as O.7 pct by volume, is shown to eliminate subcritical crack growth in gas environments caused by hydrogen or water vapor. However, dissolved oxygen in water has little or no influence upon crack-growth rates. Oxygen-stopped cracks may be restarted by water, or by hydvogen or water vapor if oxygen is removed from the environment. These observations are interpreted in terms of preferential adsorption of oxygen at the crack tip and the formation of an oxide barrier. RECENT investigations1-3 have demonstrated that environmental factors are frequently responsible for delayed failure in martensitic high-strength steels. The environment causes crack initiation from preexisting cracklike flaws at unexpectedly low stresses, often far below the uniaxial yield strength. The crack then propagates at a rate controlled by the environment and the crack-tip stress-field intensity; during this period crack propagation will cease if either the stress or the aggressive environment is removed, and this may be considered a definition of subcritical crack growth. Fracture occurs when the crack has grown to a critical length, such that the fracture toughness of the steel is exceeded. Several liquids are known to cause delayed failure, but water and water vapor are the most severely damaging of the environments investigated to date.'-3 It has been suggested that hydrogen produced during corrosion reactions may be the actual embrittling agent2 The severe embrittlement caused by water vapor inevitably raises the question as to whether other gas environments are damaging. Previous work4'5 has demonstrated that high-pressure hydrogen (2250 psi or greater) is an effective embrittling medium, as measured by such criteria as reduction in area, notch tensile strength, and time to failure. Moreover, the embrittlement was eliminated by the addition of small quantities of air or oxygen to the high-pressure hydrogen, but it was not influenced by additions of nitrogen or argon.4 In the present study attention is focused upon gas environments at atmospheric pressure, in particular hydrogen and oxygen. The influence of these constituents upon the initiation and growth of a crack from a pre-existing cracklike flaw in a high-strength steel was determined directly by the electric-potential method of monitoring crack growth. MATERIALS AND PROCEDURE The H-11 steel was supplied by the U.S. Naval Research Laboratory as 3 by 12 by 0.065 in. sheet specimens with 1-in. transverse center slots. The slot tips were finished by Elox machining to a radius of 0.001 in. or less. The yield strength was 230,000 psi; chemical composition and heat-treatment schedule are given in Table I. The experimental apparatus, precracking procedure, and incremental loading sequence have been described previously.3 In the only significant change, precracking was sometimes carried out by a hydrogen embrittlement and baking technique. All experiments were conducted at room temperature; the hydrogen gas environment was purified by a commercial palladium purifier. Crack initiation and propagation were followed by the electric-potential method,'-3 using a calibration that has been recently dicussed. Stress-field intensities at the crack tip were computed by the conventional Irwin frmula; the plasticity correction was negligible and therefore not included. EXPERIMENTAL RESULTS A striking brittleness associated with molecular hydrogen at atmospheric pressure is demonstrated by the data in Table I1 and Fig. 1, which indicate that subcritical cracks in hydrogen initiate at lower stress-field intensities and propagate more rapidly than in fully humid argon. Ki and Kf are the crack-tip stress-field intensities at initiation and termination of subcritical crack growth, respectively. Termination, of course, corresponds to fracture. In both hydrogen and humid argon Ki is less than Kf

Jan 1, 1967

By Eugene Rabinowitch

The Chemistry of Uranium. By Joseph J, Katz and Eugene Rabinowitch. Published by McGraw-Hill, Book Co. of New York, 1951. 609 P. $7.15.--This volume is the first half of a comprehensive treatise on uranium chemistry. It contains a detailed summary of the properties of the element uranium, including its occurrence in nature, extraction from ores, and the physical and chemical properties of uranium metal. Binary compounds of uranium with hydrogen, oxygen, nitrogen, and the halogens, among others, receive extensive discussion, including methods of preparation and physical properties such as crystal structure, thermochemistry and volatility. A very large proportion of the material in this volume is based on the results obtained in the laboratories of the Atomic Energy Project, much of it not published before. In addition, all of the open literature has been critically surveyed and integrated with the results of the Atomic Energy Project studies. Principles of Geology. By James Gilluly, Aaron C. Waters and A. O. Woodford. Published by W. H. Freeman & Co., San Francisco, Calif., 1951.640 P. $5.75.-This book attempts to summarize some of the knowledge that geologists have won from the study of the earth. It covers such subjects as movements of the earth's crust, records of earth movement, stream erosion and deposition, deserts, the ocean and mineral resources of the earth. The authors have concentrated on the analysis of processes that are at work upon and within the earth. rather than to present a catalog of descriptive facts and terms. The development of stratigraphy is also outlined. Pictures, maps, and tables are used to illustrate the major points of each chapter.

Jan 9, 1951

By Sidney Powers

Discussion of the paper of SIDNEY POWERS and ALFRED C. LANE, presented at the New York meeting, February, 1916, and printed in Bulletin No. 110, February, 1916, pp. 535 to 548. N. L. BOWEN, Washington, D. C. (communication to the Secretary*). -This detailed study and. complete demonstration of differentiation as a result of the sinking of crystals has a great general significance in petrogenesis. If this action can be demonstrated in an effusive body, even though a very thick one, how can one doubt its possibility in large intrusive bodies? The authors speak of the sinking of augite and the rising of plagioclase but I should consider that they should depend entirely on the former action to obtain their results. It is true that in my experiments, to which the authors refer, a floating of crystals was in one case obtained, viz., in the case of tridymite crystals, but it must be remembered that tridymite has an exceptionally low density. Plagioclase crystals, on the other hand, are of nearly the same density as basaltic liquid. Under magmatic conditions they might be a little heavier than the liquid or a little lighter, we do not know which, but the margin would be exceedingly small and any motion resulting, whether upward or downward, would be correspondingly small in the usual case. For this reason I should think that the sinking of pyroxene should be considered probably the sole factor in producing the observed result, for which purpose it appears to be entirely adequate. The measurements of grain have also a certain significance in this connection. In the experiments referred to a difference of grain was obtained in different parts of the charge, which was entirely independent of the rate of cooling but connected with the fact that a sinking crystal does not depend entirely upon diffusion for the collection of its material from the surrounding liquid. The crystals which sank a considerable distance were therefore exceptionally large. Now in the Cape Spencer flow the augite crystals are normally (top and bottom) somewhat smaller than the plagioclase crystals, but in the layer somewhat below the middle,

Jan 5, 1916