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By Leslie Burris, J. C. Hesson

The diffusivity of uranium in liquid cadmium has been measured as a function of temperature by the capillary -bath technique. The diffusivity measurements were made at 4509 500°, 575º, and 650°C, over which temperature range the diffusivity of uranium varied from 1.3 to 2.3 x 10-5 sq cm per sec. The diffusivity of uranium in cadmium was less than that predicted by the Einstein-Stokes equation. VERY little information is available on the diffusivity of uranium in liquid metals. Bonillal has reported a single measurement of the diffusivity of uranium in bismuth. Measurement of the diffusivity of uranium in cadmium was undertaken, not only to supply data in an area in which a dearth of information exists, but also because of a need for this physical property measurement in connection with mass transfer studies now underway in the U-Cd system at Argonne National Laboratory. The capillary-bath method used in this work has been successfully used by other workers2"4 to obtain diffusivities in liquid metal systems. Although considerable experimental technique is required to obtain reliable diffusivity measurements, the basic information required is only that of temperature, capillary tube length, the initial and final compositions of the alloy in the capillary tube, and the composition of the bath into which the solute element is diffusing. From these measurements, diffusivities may be calculated using Fick's law. The diffusivity equations are presented in the Appendix. Equations which are often used to predict diffusivities in dilute solutions5 are the Einstein-Stokes equation: D= (kT)/(6pµr) and the Eyring equation: D = (?,kT/?y?zp), where D= diffusivity (sq cm per sec), k = Boltzman's constant, T= temperature ("K), p = viscosity (poises), r = radius of diffusing molecule or species (cm), and A,, Ay, and A, are the diameters of the diffusing molecule in the three axial directions. For round molecules, the Eyring equation gives values which are 37r times larger than the Einstein-Stokes equation. In this work, the experimental values were compared to the Einstein-Stokes equation. Experimental values of diffusivities in liquid metal systems usually lie between those predicted by the Einstein-Stokes and Eyring equations. The viscosity values for cadmium were obtained from the Liquid Metals Handbook.6 EXPERIMENTAL APPARATUS AND PROCEDURE The general procedure employed consisted of rapidly immersing in a molten cadmium bath containing a negligible amount of uranium a capillary

Jan 1, 1963

By d&apos, C. Antonio, S. H. Reichman

In the course of our studies of the annealing behavior of vapor-deposited silver films we have determined the electrical resistivity as a function of annealing temperature for films in the thickness range of 630 to 3240A. Fig. 1 shows the resistivity of the silver films vs film thickness in as-deposited and annealed conditions. The films were prepared by depositing 99.999 pct pure silver from molybdenum boats onto Vycor substrates. Deposition was conducted at a residual pressure of 5 x 10"6 Torr at rates of 20 to 408, sec-'. Thicknesses were determined using a multiple-beam interferometer. During annealing, resistance was measured using the four-probe method. Measurements were made every 5°C during two consecutive anneals to 300°C under a continuous vacuum of 2 x X6 Torr. The heating and cooling rates during annealing were approximately l° and 2°C min-', respectively. Typical resistivity vs temperature curves are shown in Figs. 2 through 4. There is an inflection point evident at 120°C on Fig. 2, the first anneal of a 3240A film. This inflection point was found on all films above approximately 1!00A on both first and second anneals. Below 1400A the inflection occurred at approximately 180°C. Figs; 3 and 4 show the first and second anneals of a 1370A film. The inflection point occurs at 180°C on the first anneal and approximately 120°C on the second. Our interpretation of this phenomenon is based on oxygen liberation from the film surface. It is well-documented that the presence of oxygen on silver surfaces causes a reversible increase in resistivity.1"3 The liberation of this oxygen, for example during vacuum annealing, would therefore cause a decrease in resistivity as observed on Figs. 2, 3, and 4 as a change in slope. This is accounted for by the decomposition of Ag20 on the film surface. The free energy of AgzO becomes positive between 125" and 225°C.4 The thickness dependence of the inflection points can be explained as an orientation effect. The films used in this study were preferentially oriented with their (111) planes parallel to the Substrate.''~ In addition it has been sten that the thinner films, below approximately 1500A, possess a decided "hill and valley"

Jan 1, 1969

By P. C. Johnson, B. A. Stein

This paper describes a study of the effects of combined heat treatment and explosive loading on the mechanical properties of high-strength steels. nis program investigated two distinct areas: 1) the effect of shock waves, without gross irreversible defmmution, on a 3-Cr steel at various stages of heat treatment; and 2) the effect of rapid deformation (explosive forming) on H-11 and D6-AC steels in the metastable austenitic state. The mechanical properties of these steels were improved, in some cases markedly, as a result of these treatments. ,AUSFORMWG, which requires the plastic deformation of metastable austenite, is a process which can appreciably improve the properties of selected alloy stee1s.l,2 The Ausform process significantly increases the strength of these steels without decreasing their ductility. The properties at high temperatures are also improved through a change in the response of the steels to tempering. Although the mechanism by which ausforming alters the properties of these steels is not fully understood, it appears that the dislocation arrays produced by deformation of the metastable austenite influence the structure of the martensite on subsequent transformation. This, in turn, affects the strength, ductility, and tempering response of the martensite. This research used chemical explosives to deform steels at various stages in their heat treatment in order to improve the properties of these steels. The explosive energy is used in two ways; 1) high-pressure shock waves are propagated through the steel to produce extensive microscopic shear strain without causing a large irreversible change in shape, and 2) explosive energy is used to cause extensive macroscopic plastic strain in the metastable austenitic state (explosive forming). I) AUSFORMING WITH INTENSE SHOCK WAVES The steel used in this phase of the research was an alloy having a nominal composition 0.43 pct C, 3.0 pct Cr, 1.5 pct Ni, and 1.5 pct Si. The steel was subjected to intense shock waves in three conditions: 1) in the metastable austenitic state, 2) in the tempered mar tens itic state, and 3) in the tempered martensitic state after ausforming by conventional techniques. The specimens were in the form of disks 2.75 in. in diam and 5/16 in. thick. These were incorporated into a specimen assembly consisting of two disks pressed into a 5 by 5 by 1 in. block of stainless steel, Fig. 1. Spalling (or scabbing) is confined to the front disk. The specimen is protected from oxidation and decarburization by the surrounding metal. The temperature of the assembly is monitored by a thermocouple inserted into one side of the stainless steel block. The assembly is positioned over an oil reservoir which serves both as a means of catching the disks and as quenching medium for the disks shocked under ausforming conditions. Plane shock waves are introduced into the assembly by a metal driver plate impacting the top surface of the block. The driver plate is accelerated by a chemical explosive sheet supplied by E. I. du Pont de Nemours & Co. All the specimens were subjected to plane shock waves having a peak pressure of approximately 430 kbar. The pressure is that quoted by G. E. Dieter for the plane wave generator used in this work.' The driver plate used was 1/4 in. thick, so that the initial pulse was essentially a l/2-in.-wide square wave. The attenuation of the peak pressure during the subsequent 1/4 in. is estimated to be less than 5 pct. The shock front induces a temperature rise, a portion of which is irreversible. Rough estimates (+25 pct) of this temperature rise have been made for iron shocked at room temperature.4 For a 500-kbar shock wave, the temperature rise in the shock front is about 700°F, and is held for a time of the order of microseconds. The irreversible temperature rise, which remains after the shock wave passes, is about 450°F.4 The disks are quenched to room temperature within a few seconds of the shock treatment. It should be emphasized that the temperature rises given above are estimates for pure iron at room temperature, and are not necessarily true for the tests made in this work. The disks shocked at temperatures in the metastable austenitic range were austenitized in the stainless steel assembly in a furnace protected from the firing area. The assembly was removed from the furnace and placed over the recovery reservoir. The plane wave generator was then positioned and

Jan 1, 1963

By William Cruger

OUTLINE SUMMARY A. Brief Description B. Characteristics 1. Can be highly cost effective 2. Restricted in usage 3. Political Controversy 4. Volume of Transactions 5. Users C. Mechanism 1. Five steps D. Investor issues 1. Application 2. Restricted usage 3. Discount 4. Formal or informal process 5. Restricted benefits 6. Recompense 7. Window of opportunity THE VARIOUS PROGRAMS1 A. Brazil B. Chile C. Venezuela D. Argentina E. Mexico USAGE IN THE MINING, METALLURGICAL, AND PETROLEUM INDUSTRIES

Jan 1, 1990

By Thomas J. Ferree

The principle mineral concentration practices today can be divided into three basic process categories: magnetic separation, flotation and gravity separation. The basic processes have been in use for many years with only limited changes occurring in equipment design or process technique. In general, equipment and process techniques have been altered only after a need for change has developed. With exceptions for changes necessitated by new environmental laws, most equipment and process improvements have evolved in accordance with the desire to concentrate larger quantities of material at lower costs. The basic result has been the development of larger capacity equipment, to wit: larger flotation cells, larger blast furnaces, larger haulage equipment and larger chemical process equipment. However, there has been practically no changes in the size of spirals, tables, jigs, or-within limits- magnetic separators. (The exception being high-intensity magnetic separators). Consequently, a "new" device has entered the scene which may fill a void in the gravity separation field. It is called a Reichert cone concentrator.

Jan 3, 1973

While mining silver at Butte in 1882, Marcus Daly is reputed to have told his partners in The Anaconda Silver Mining Co., "It looks rather gloomy. The vein is running into copper." Recently, The Anaconda Co. authorized an $11 million expenditure to be made over the next five years to ensure their "running into copper" at deep levels for many more years. The new development program is designed to permit both deeper and more widespread selective mining in "the richest hill on earth" by means of additional shaft-sinking, reactivating closed mines, and establishing new haulageways and centralized hoisting facilities. Historically a deep level selective mining camp, Butte will now continue its uncommon use of three main types of mining methods at one camp-selective mining, block caving, and open pit mining. It was thought by some people that the construction of the Kelley shaft and the subsequent beginning of block caving operations in 1952-outgrowth of the Greater Butte Project-signaled the end of stope mining of high-grade ores at depth. This feeling became more pronounced when, in 1957, the Berkeley open pit commenced operations. During recent years, the tonnage of ore mined selectively underground has decreased, but the new program will maintain the position of selective underground mining in the overall picture of the Butte operations for many years to come.

Jan 7, 1960

By W. C. Thurber, C. J. McHargue

THE deformation textures of metals have been extensively studied because of both the practical implications in metal fabrication and the fundamental insight into the behavior of the metal during deformation. Most studies have been concerned with pure metals or solid-solution alloys and relatively little attention has been directed toward more complex alloy systems. Barrett' and Brick2 have summarized work on multiphase systems in terms of the relative ease of deformation of the phases. Thus, if the phases are deformed about equally, each develops its usual texture for the particular fabrication process. This behavior has been reported for Ag-Cu and Cd-Zn alloys3 and 62-38 brass.4 A dispersion of hard particles in a softer matrix interferes with the normal reorientation of the matrix lattice during deformation, thus distorting the texture or in some cases preventing its development. Increasing the amount of carbon in steel has been observed to increase the randomness of the ferrite5 and almost random textures have been reported for A1-12 pct Si eutectic alloy wires.6 It has also been noted that if the second phase is platelike, deformation causes the platelets to line up in a common direction. The present work concerns a quantitative study of the deformation textures in aluminum-uranium alloys containing 5 or 13 wt pct U. Alloys in this composition range are characterized by a pure aluminum matrix in which the intermetallic compound UA14, is dispersed. From a fundamental standpoint, this system affords the opportunity for studying the effects of a dispersed phase on texture development in an essentially pure metal matrix. Further, these alloys are commonly used as fuels for nuclear research and testing reactors, and a knowledge of the preferred orientation may be useful in evaluating physical and mechanical properties as well as response to fabrication. The deformation textures in sheets of aluminum (99.996 pct), Al-5 pct U alloy, and Al-13 pct U alloy were determined for reductions in thickness of 90 pct by cold rolling. The texture in an alloy rod of the latter composition which had been extruded at 455°C was also determined. It can be readily ascertained from the aluminum-uranium phase diagram that the 5 pct U alloy is hypoeutectic and contains 7.3 wt pct (3.4 vol. pct) UAl4. The 13 pct U alloy has the eutectic composition and contains 18.9 wt pct (9.4 vol. pct) UAl,; however, because of nonequilibrium solidification conditions, the typical eutectic microstructure was not developed. The alloys were prepared by open-air melting in graphite crucibles. The slab castings were cropped and cold reduced 90 pct in thickness on a two-high mill. The slabs were reversed after each pass. Although the uranium-bearing alloys exhibited edge cracking, they could be cold rolled to the desired thickness. Small coupons 1.5 by 0.75 by 0.1 in. thick were sheared from the center of the rolled plate with a major axis parallel to the rolling direction. To obtain a specimen of sufficient thickness for machining of the X-ray diffraction specimen, three coupons were laminated into a single three-ply sandwich with a suitable adhesive. Adhesives which could be cured at room temperatures were selected in order to prevent recrystallization during bonding. Bondmaster M-648 (Rubber and Asbestos Corp.) was used for the pure aluminum laminate and Armstrong A-6 (Armstrong Products Co.) was used for the alloys. The alloy for extrusion was cast in a cylindrical graphite mold! cropped and machined into a 3-in. diam by 4-in. long billet. This billet was preheated to 455°C, upset to 3.125 in. diam, and extruded on a 700-ton hydraulic press at a speed of 6 fpm through a flat-face, 1-in. diam die. The rod was quenched with a water spray as it emerged from the die. Pole-distribution data were obtained using the diffractometric method described by Jetter and Borie.7 A spherical X-ray diffraction specimen of

Jan 1, 1961

By F. M. Lewis, Johnson. E. C.

BY now application of the liquid-solid cyclone to various classification problems in the chemical and metallurgical fields is more or less familiar. A less publicized application receiving wider consideration as time goes on is its use as a classifier in closed-circuit grinding operations. This paper presents the costs involved and the experience gained from operating a unit of this kind. In May 1951 the Tennessee Copper Co. installed in its London mill at Copperhill, Tenn., a liquid- solid cyclone in closed circuit with a 6x12-ft ball mill. The circuit in which this cyclone is used is the regrind or secondary grinding circuit of a copper flotation plant. Originally it consisted of a 7x1-ft conical ball mill in closed circuit with a bowl classifier. Changes made in the primary grinding circuit of the mill necessitated a regrind circuit of greater capacity. The bulk concentrate to be ground was raised from 900 or 1000 tpd to 1200 or 1300 tpd, and to accommodate this increase a 6x12-ft ball mill which had been in the primary grinding circuit was moved into the regrind circuit. When this was done it was found that the classifier was too small to give efficient operation. Space in the plant was at a premium, and since use of the cyclone offered considerable economy the installation shown in Figs. 1-3 was made.

Jan 6, 1954

Jan 1, 1939

Jan 1, 1939

Jan 1, 1914

By Robert C. Weed

Leaching in place at Cananea began in the 1920's on a limited scale. The first plants were small wooden boxes located underground in the Capote and Oversight mines, and output was low. Scrap iron was used as precipitant. Later several other small plants were started up. Leaching was limited entirely to underground areas, and production remained low. The Veta precipitating plant, the first on a larger scale, was put into operation in the late 1920's. After a period of intermittent service it was rebuilt in 1946 and has since been running continuously.

Jul 1, 1956

By AIME AIME

COUNCIL* PRESIDENT OF THE COUNCIL. JAMES F. KEMP NEW YORK, N. Y.. (Term expires February, 1913.) VICE-PRESIDENTS OF THE COUNCIL. S. B. CHRISTY BERKELEY, CAL. R. V. NORRIS WILKES-BARRE, PA. GARDNER F. WIILLIAMS WASHINGTON, D. C. (Term expires February, 1913.) . KARL EILERS NEW YORK, N. Y. WALDEMAR LINDGREN WASHINGTON, D. C. BENJAMIN B. THAYER NEW YORK, N. Y. (Term expires February, 1914.)

Jul 1, 1912

By Donivan L. Gordon, Fred H. Dorheim

Often, as viewed by the public and many in the mining industry, abandoned limestone and gypsum quarries offer a simple, economic solution to the twofold problem of solid-waste disposal and land reclamation. In a state where about 75% of the existing quarries are in hydrologic connection with carbonate aquifiers the rationale for considering the storage of solid waste in them must be critically examined. Consistent with the requirements of water resources protection, criteria are suggested to evaluate the potentiality of using abandoned limestone and gypsum quarries as sanitary landfill sites.

Jan 1, 1975

By J. A. B. Forster

The operations of the Electrolytic Zinc Co. of Australasia Ltd. involve the preliminary roasting of zinc concentrate from Broken Hill, New South wales, at a number of acid-making centers on the Australian mainland. The partially roasted material is shipped to the Tasmanian plant where it was formerly re-roasted prior to leaching,' but this practice was gradually abandoned in favor of the flotation of leach residue for the recovery of a concentrate containing about 22 pct sulphide sulphur and known as secontlary or Risdon concentrate.2 This change, together with increased zinc production, called for new furnaces at Risdon for the roasting of 10-50 tonst of secondary concentrcite and 90 tons of new concentrate per day. The war situation made it imperative that construction be commenced without delay and to save time it was decided to base the design on that of Skinner type furnaces which had been built in South Australia twenty years earlier. This involved some sacrifice of desirable features but did not prevent the incorporation of provisions which had enabled small Herreshoff type furnaces to roast secondary concentrate autogenously. The roasting rate in existing furnaces was 10-12 Ib sulphide sulphur per sq ft of hearth area per day, and eleven hearths, 20 ft in diam, were provided in the two new furnaces in anticipation that they would prove capable of the autogenous roasting of 130-140 tons of concentrate per day from 28-29 pct sulphur down to 4.5-5 pct, with an oxidation rate of 11-11.5 lh S/S per sq ft of hearth area per day. It was soon realized, when the first of the furnaces went into operation, that a much better performance than this might be given, and the purpose of this paper is to show how a treatment rate of 100 tons per furnace day, and oxidation rates approaching 15 lb S/S per sq ft per day have been reached. Furnace Design General specifications for the design were based on the results of experience with several other types of furnace and on the special operating conditions

Jan 1, 1950

By John V. Beall, John Cameron Fox

Organization In 1948, the Committee on Divisionalization and Publication Program of AIME, known as the Johnson Committee, recommended the reorganization of the Institute into three branches, Mining, Metals and Petroleum. This recommendation was accepted and the new organizational structure was implemented in Jan., 1949. The Mining Branch, at the time of the formation, had three divisions: the Coal Division formed in 1929, the Industrial Minerals Division (IndMD) dating from 1935, and the Minerals Beneficiation Division (MBD) formed in 1948 from the Milling Methods Committee, which had existed for many years. There did not exist, however, a division for the geologists and mining engineers. From the time of the founding of the Institute, this group was the main stem of AIME and never felt the need to segregate. The disciplines of mining and geology were served by a number of technical standing committees of AIME. With the birth of the new Branch, a new Division, the Mining, Geology and Geophysics Division (MGGD) was formed, completing the divisional structure of the Mining Branch and providing a home for all members. The governing body was the Mining Branch Council, with two members from each Division of the Mining Branch and one each from the Mineral Industry Education Division and the Mineral Economics Division. These last two divisions served all three Branches of AIME. The Division is such an important unit in the organization structure that it is of value to explain that it appoints committees to handle pro- grams, publications, and awards - representing the main functions of the Institute - as well as many others. There is enough flexibility in the organization so that each Division may have its own special committee structure as long as primary functions are provided. The past is indeed prologue to the future, for in 1957 the Johnson "Branches" gave way to the Fletcher "Societies." The Fletcher Committee, in 1958, recommended a new reorganization into Societies, each with the authority to administer its own finances and to designate certain officers and directors to the AIME Board. The date on which the Society of Mining Engineers was formed in Feb., 1957, has become known as "R" Day. A smooth transition from the loose Branch structure to Society organiza-

Jan 1, 1971

By F. F. Craig

The authors have done a commendable job in combining a number of recognized waterflood performance prediction methods into one composite method. The availability of a FORTRAN program for this composite method should encourage its widespread industry use. Pan American has had a computer program developed along similar lines for a number of years,' and it has received more use than any other reservoir prediction method. In three important stages of a pattern waterflood, the authors fail to consider fully the effects of water-oil mobility ratio on performance. This is discussed in the following paragraphs and modifications of the prediction method are suggested. During the early stages of a waterflood in a partially depleted formation, the injected water and its preceding oil bank move out radially from the injection wells. As pointed out in the author's paper the method of Yuster and Calhoun2 or predicting the water injection rate during this period assumes that the mobilities of the water and oil are equal. In his book, Muskat3 resents a modification of the Yuster-Calhoun approach that considers fully the influence of water-oil mobility ratio. In Muskat's method, the prediction of the injection rate-injected volume-time relationship is expressed in readily programmed dimension-less unts. At and following fillup the five-spot pattern consists of a water-invaded pattern with the remainder of the pattern containing only oil and connate water. In the paper, Eq. 18 is used to calculate the water injection rate at fillup. This equation considers that the entire pattern is invaded by water. To properly consider both the incomplete areal sweep of water and the water-oil mobility ratio, Eq. 18 should read:

Jan 1, 1969

By AIME AIME

On Nov. 11, 1909, M. Alexandre Pourcel, of Paris, France, upon the proposal of a large number of distinguished members, and the unanimous recommendation of the Council, was elected by the Board of Directors an Honorary Member of the Institute. M. Pourcel has devoted forty-three years to the metallurgy of iron and steel ; and the work which he did between thirty and forty years ago constitutes an important part of the founda¬tion of the practice of to-day. Among his striking contribu¬tions are : (1) his perfection, in 1869, of the manufacture of high-grade ferro-manganese in a carbon-lined open-hearth furnace, instead of the costly crucibles previously used; (2) his discovery, in 1874, of the method of making solid steel cast¬ings; (3) his manufacture, in 1875, of ferro-manganese and silico-spiegel in the blast-furnace; and (4) his anticipation, in 1875, of modern American blast-furnace practice, by the pro¬duction, in a very small furnace, of Bessemer pig containing 2.5 per cent. of silicon, from a burden yielding only 46 per cent. of iron, and with a consumption, per ton of pig, of only 1,8401b. of coke, containing 15 per cent. of ash. These brilliant pioneer achievements, together with his contributions to cur¬rent technical literature, won for him the Bessemer gold medal of the Iron and Steel Institute ; the great" medal of honor," which is the highest award of the French Society of Mineral Industry, and other gold medals, as well as the distinction of honorary membership of the Comité des Forges de France, which was conferred upon him in 1891. In recent years, M. Pourcel has been instrumental, as consulting engineer of the Société de Commentry-Fourchambault, at Decazeville, France, in an extraordinary development of the manufacture of special steels. The Invar plant, of this company, is said to make a greater variety of such steels (includ-

Dec 1, 1909

By Che-Yu Li, J. L. Gregg, W. F. Brehm

Oriented, oxygen-doped niobium bicrystals were tested in liquid lithium. The grain boundaries were attacked preferentially. The depth of the penetrated zone varies as (time)2. The penetration was aniso-tropic, had a high activation energy, and increased with the increased oxygen doping level. A possible model was proposed to account for the experimental observations. 1 HE grain boundary penetration of a metallic system by liquid metal has been studied by several investigators. Their results are summarized by Bishop.' Most of these works show that the penetration by liquid metal corresponds to the phenomenon of liquid metal wetting. In the case of a grain boundary, wetting will occur when twice the solid-liquid interfacial tension is smaller than the grain boundary tension resulting in the replacement of the grain boundary by two new solid-liquid interfaces. Other possibilities exist; for example, the atoms of the liquid metal may diffuse into the grain boundary region due to chemical potential gradient. The gradient can be produced by impurity segregation or simply be due to the increase in solubility in the grain boundary region. The penetrated grain boundary in these cases may remain solid at the test temperature. The Nb-Li system has been of considerable interest because of its possible technological applications. For fundamental interest it provides a possibility of studying the grain boundary penetration process which is not controlled by the wetting mechanism. The pure niobium is not attacked by the liquid lithium, but if niobium containing more than 300 to 500 ppm oxygen by weight is exposed to liquid lithium, corrosion occurs at the solid-liquid interface and preferentially at grain boundaries. Previous investigators2-' have proposed that this preferential corrosion at grain boundaries is caused by oxygen segregation there, with subsequent inward diffusion of lithium to form a Li-Nb-0 compound. These investigators also found that the corrosion could be retarded by adding 1 pct Zr to the niobium to precipitate the oxygen as ZrO2 upon proper heat treatment. However, there are no quantitative data on the kinetics of the grain boundary penetration process to test the validity of the proposed corrosion mechanism. In this work an investigation of this penetration process in oriented bicrystals was made as a function of the oxygen doping level in the bulk niobium and the grain boundary orientation. A possible model for the penetration process based on the experimental results was proposed. EXPERIMENTS Oriented niobium bicrystals were grown by arc-zone melting oriented single-crystal seeds.7 These bicrystals contained simple tilt boundary. The [001] directions in the two grains were tilted about a common [110]. The bicrystals were 31/2 in. long and 5 by 4 in. in cross section with the straight, symmetric, planar grain boundary longitudinally bisecting the crystal rod. The bicrystals were doped with oxygen by anodically depositing a layer of Nb2O on the surface in a 70 pct HNO solution at 100 v, using a stainless-steel cathode. The specimens were homogenized by annealing in evacuated quartz tubes at 127 5°C. Oxygen content of the niobium was measured from microhardness values, after DiStefano and Litmman.' Supplementary checks were made with vacuum-fusion analysis.7 Individual test specimens cut from the doped bi-crystal rods, about by by % in. in size, were tested inside double jacket sealed capsules. The inner jacket was niobium, the outer was stainless steel. The niobium inner jacket eliminated the problem of dissimilar-metal mass transfer.' The lithium (99.8 pct pure, obtained from Lithium Corp. of America) was handled only in a purified argon atmosphere in a Blickman stainless-steel glove box. After introduction of lithium, the capsules were sealed by welding. Further detailed experimental procedures are given in Ref. 7. The capsules were heat-treated in vertical Marshall resistance furnaces. Temperatures were controlled to When heating above 1100°C, it was necessary to seal the furnace work tube and flow argon through to prevent failure of the stainless-steel outer jacket of the capsule. Tests were made on 6" 2", 16" 2, and 33" i2" bicrystals at oxygen levels up to 2600 ppm by weight in the 6' and 16" crystals and with 1300 ppm oxygen in the 33' crystals. The oxygen levels were controlled to 100 ppm. Most of the quantitative data were obtained from 16" bicrystals between 800" and 1050°C. The capsules were quenched into water after the test and cut open with a water-cooled abrasive wheel. The capsules were then submerged in water, which dissolved the lithium and freed the specimen. Measurement of the depth of the penetrated zone in the grain boundary was done either on metallographically prepared surfaces or directly on the grain boundary plane after the specimen was fractured in tension in the grain boundary plane. The depth of penetration measured by both methods agreed well. Further details describing these techniques have been reported elsewhere.'p7

Jan 1, 1969

By Charles C. Hawes

DETERMINATION OF SILICA OXIDE iron ores usually are found in intimate association with silica and phosphorus compounds. Their quantitative separation and purification sometimes present difficult problems to the chemist. Silicic acids may represent various degrees of dehydration. They are exeedingly weak, but combine with metallic oxides and form some of the most stable oxides in nature, the silicates. When iron ores are treated with hydrochloric acid, they yield practically all their iron. However, apart from rare exceptions, varying amounts of insoluble residues of silica, alumina, lime, magnesia and compounds of phosphorus, sulphur, titanium, chromium and others will be left. If the oxides of silicon, aluminum and titanium are present in small quantities, the insoluble residue is generally very small, but the presence of these oxides is more usual in larger quantities. Therefore, only a special treatment can break the bond between these elements. Ore Residues Acids remove the soluble constituent of the ore, leaving the insoluble residue, which chemically is rock or gangue and must be treated accordingly. Alkali carbonates are used frequently to break up the residue, but other fluxes have also been recommended, such as a number of lead and boron salts. The introduction 0f these salts, which offers certain advantages, requires, however, their removal before the other constituents can be analyzed, and this elimination is sometimes difficult. Usually in quantitative analysis silicates are dissociated by fusing them in a platinum crucible with sodium carbonate, thereby forming sodium silicate, Na2SiO3, sodium aluminate, Na2Al204, sodium titanate, Na2TiO3, and carbonates of other elements. All the carbonates are soluble in hydrochloric acid, but also some silicic acid is formed that must be rendered insoluble. To this end the solution is evaporated several times, as the first evaporation still leaves as much as 5 per cent of the silica soluble. Even after a number of evaporations, minute quantities of silica may be found with the iron and alumina present. Perchloric Acid as an Agent for Dehydrating Silicic Acid Perchloric acid, HC104, (60 per cent), has been used for years as a solvent, but few chemists have used it to dehydrate silica. It is derived from anhydrous perchloric C1207, which is most unstable and dangerous. Perchloric acid is a strong oxidizing agent, which boils at 203°C. It is more effective in rendering silica insoluble than any other known agent, and most rapid in action. After perchloric acid is added to a mixture containing silicic acid, the resultant solution is

Jan 1, 1945