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By George E. Moore, B. K. Miller

The Missouri fire clays are here divided into plastic and semiplastic clays occurring as widespread bedded deposits in east central Missouri and flint and diaspore clays occurring as isolated "sink-hole" deposits in the north central Ozark region. Visual inspection was the first method used in clay prospecting. Thin overburden, hard sandstone "rimrocks," and the occurrence of diaspore float made this method particularly applicable in the flint and diaspore fields. The first drilling tool used was a hand auger. One man can drill 25 to 50 ft. per day at a cost of about 35 cents per foot. Holes can be drilled to a depth of 150 feet. Spud drills are often used where the overburden is hard. This drill uses a slotted earth socket bit. A two-man crew can drill about 100 ft. per day at a cost of about 35 cents per foot. Mechanically powered auger drills have been used extensively in wildcat drilling in the past few years. This type of drill furnishes a continuous set of cuttings. The practical depth limit with this drill is 50 to 60 ft. Two men can drill 300 ft. per day at a cost of about 20 cents per foot. Core drilling is used mainly to prove a known 'lay deposit. A A crew with a No. 22 Sullivan drill can drill about 30 to 40 ft. per day in soft clay, at a cost of about $1.25 per foot. Introduction Because of the geological variations in the Occurrence of the several types of fire clay mined in Missouri, it is necessary, when discussing the prospecting methods used for discovering and proving these clays, to divide these operations into two classes, one including plastic and semi-plastic fire clays, the other flint and diaspore clays. The plastic and semiplastic fire clays in the east central and St. Louis districts are generally classified as Cheltenham clays. This formation is a more or less continuous deposit and is found Over a large area in east central Missouri. There are variations, however, in the quality and thickness of the clay, which necessitate detailed prospecting in order to determine deposits of economic value. The nature of the overburden (Fig. 1), which consists of Pennsylvanian limestone and shale beds of varying thicknesses, and a mantle of glacial drift, regu1ates the methods and equipment used in prospecting for these clays. The district in which these clays occur is a gently rolling upland region, characteristic of most of northern Missouri. Along the southern fringe of this area there are numerous deposits of flint clay lying as masses or lenses in depressions at the base of the continuous and widespread Cheltenham formation, or as outlying "sink-hole" deposits in the area marginal to that formation. South of the Missouri River in the north central Ozark region, there are high-grade flint and high-alumina clays, commonly referred to as burley and diaspore clays in sink-hole type deposits. The overburden On these deposits is thin, consisting chiefly of soil and hard-pan, which varies from a plastic

Jan 1, 1948

By B. K. Miller, George E. Moore

The Missouri fire clays are here divided into plastic and semiplastic clays occurring as widespread bedded deposits in east central Missouri and flint and diaspore clays occurring as isolated "sink-hole" deposits in the north central Ozark region. Visual inspection was the first method used in clay prospecting. Thin overburden, hard sandstone "rimrocks," and the occurrence of diaspore float made this method particularly applicable in the flint and diaspore fields. The first drilling tool used was a hand auger. One man can drill 25 to 50 ft. per day at a cost of about 35 cents per foot. Holes can be drilled to a depth of 150 feet. Spud drills are often used where the overburden is hard. This drill uses a slotted earth socket bit. A two-man crew can drill about 100 ft. per day at a cost of about 35 cents per foot. Mechanically powered auger drills have been used extensively in wildcat drilling in the past few years. This type of drill furnishes a continuous set of cuttings. The practical depth limit with this drill is 50 to 60 ft. Two men can drill 300 ft. per day at a cost of about 20 cents per foot. Core drilling is used mainly to prove a known 'lay deposit. A A crew with a No. 22 Sullivan drill can drill about 30 to 40 ft. per day in soft clay, at a cost of about $1.25 per foot. Introduction Because of the geological variations in the Occurrence of the several types of fire clay mined in Missouri, it is necessary, when discussing the prospecting methods used for discovering and proving these clays, to divide these operations into two classes, one including plastic and semi-plastic fire clays, the other flint and diaspore clays. The plastic and semiplastic fire clays in the east central and St. Louis districts are generally classified as Cheltenham clays. This formation is a more or less continuous deposit and is found Over a large area in east central Missouri. There are variations, however, in the quality and thickness of the clay, which necessitate detailed prospecting in order to determine deposits of economic value. The nature of the overburden (Fig. 1), which consists of Pennsylvanian limestone and shale beds of varying thicknesses, and a mantle of glacial drift, regu1ates the methods and equipment used in prospecting for these clays. The district in which these clays occur is a gently rolling upland region, characteristic of most of northern Missouri. Along the southern fringe of this area there are numerous deposits of flint clay lying as masses or lenses in depressions at the base of the continuous and widespread Cheltenham formation, or as outlying "sink-hole" deposits in the area marginal to that formation. South of the Missouri River in the north central Ozark region, there are high-grade flint and high-alumina clays, commonly referred to as burley and diaspore clays in sink-hole type deposits. The overburden On these deposits is thin, consisting chiefly of soil and hard-pan, which varies from a plastic

Jan 1, 1948

By D. J. Brown

Froth flotation is now used to recover millions of tons of fine coal,(-1/2 mm), every year. For example, in Great Britain, 4-million tons of flotation concentrate was produced in 1960, about 3% of the mechanically cleaned out- put and 2% of the total salable output. Coal flotation is not so widely practiced in the U. S. as it is in Europe since much American coal occurs in thick seams of high grade and does not require cleaning. However, in the U. S., as elsewhere, the increasing mechanization of coal mining machinery has lead to a lowering in size and grade of product from the mine and to an increasing need for cleaning of coal to improve the grade before sale. With an increasing proportion of fines in the product, froth flotation has assumed a greater importance as a cleaning process for coal. In the last three years, over 40 flotation plants have been put into operation in the Appalachian area of the U. S.80 Fine coal recovered by means of froth flotation may be used as a powdered fuel alone or mixed with coarser grades. The removal of this fine coal from washery water makes possible the recirculation and re-use of the water and also leads to improved and more consistent operation of jigs and other separating machines which function less effectively when there is a build-up of fine solids in the washery water. Finally, froth flotation is of assistance in the production of a clarified effluent which may be discharged from the washery without polluting local rivers, streams, or wells. The 1961 cost of installing a new coal flotation plant in Great Britain would be about $19,000 per ton of dry solids input per hour, including the cost of new buildings and coal and shale filtration and water clarification equipment. The figure for the gravity concentration of the large coal, the main plant, would be about $4,800 per tph. The operating cost for the new coal flotation plant would be about $1.10 per ton. Even at this level of cost the cleaning operation is economic in Great Britain for coking coals. In the U. S., a froth flotation cost of 14$per ton of cleanfilter cake was quoted early in 1958 for one operation,l though admittedly this was a special case. Assuming a cake moisture con- tent of 30%, it is estimated that this cost is equivalent to a figure of 256 per ton of dry solids input, for the incorporation of coal flotation in an existing washery. A cost oh 416 per ton of concentrate was quoted76 in a recent analysis of flotation economics, this cost being brought up to $1.11 per ton after payment of royalty, welfare and association dues and taxes. Capital cost was $120,000 for a plant producing 133 tpd of concentrate. Before considering the treatment of coal by flotation it is appropriate to survey some of the properties of coal which are of importance in the process.

Jan 1, 1962

By F. E. Rizzo, L. R. Bidwell, D. F. Frank

THE poor high-temperature oxidation resistance of the refractory metals becomes an important problem as higher operating temperatures are sought. A meaningful analysis of their oxidation behavior requires a knowledge of the phases that can appear during oxidation as well as their relative stability. Although several extensive investigations have been carried out to obtain this information for the W-0 system,1-10 serious inconsistencies still remain. First, the standard free energies of formation (AG°) determined in recent studies which used the solid electrolyte galvanic cell technique6,7,9 differ significantly from those obtained primarily from gas equilibration measurements.1,3,4,10 The disagreement is especially large for the highest oxides. These data have been used to predict the decomposition temperatures of WO2. 72 and WO2.90.1 A considerable extrapolation is required, resulting in a large uncertainty in the decomposition temperatures. Second, Bousquet and perachon3 have presented convincing evidence, ob- tained by gas equilibration measurements, in support of the long-contested existence of W30. Phillips and chang,ll on the other hand, were not able to observe this phase under similar experimental conditions. The purposes of this work, which is part of a continuing investigation of the W-Mo system, were to resolve the discrepancies between the AGO measured by gas equilibration and solid electrolyte galvanic cell techniques, to extend the latter measurements to lower temperatures, to redetermine the WO2.72 and WO2.90 decomposition temperatures, and to apply the more sensitive electromotive-force method to the question of the existence of W3O. I) EXPERIMENTAL PROCEDURE The measurement of ?G° of reaction by the use of calcia-stabilized zirconia solid electrolyte galvanic cells has been described previously.12 The method is based on the measurement of the difference in chemical potential of oxygen between an electrode containing the two oxides of interest and a reference electrode of known oxygen activity. Two different types of cell holders were used in this study. The first type of apparatus has been described earlier." It consisted of two solid electrodes separated by a disc of electrolyte. Both electrodes were exposed to the same stream of purified helium. With this design a gaseous transport of oxygen between the two electrodes is possible. The second type of apparatus, which has also been described earlier,14 effectively separated the two electrode atmospheres. It utilized a closed-end impervious, calcia-stabilized zirconia tube that was open to the atmosphere. The tube served as an electrolyte for the cell and provided a means for separating the anode compartment, which was held under a static vacuum, from an air reference cathode. The cells and reactions of interest are described in Table I. High-purity tungsten metal was obtained from the Fansteel Metallurgical Corp. and the Allied Chemical Corp. Table II contains an analysis of each material. WO3 was prepared by oxidizing the metal in air at approximately 600°C in high-purity recrystallized alumina boats and by the dehydration of reagent-grade tungstic acid in alundum boats. The two methods of preparing WO3 resulted in slightly different purities.

Jan 1, 1968

By I. E. Campbell, R. I. Jaffe

Oxygen, nitrogen, and hydrogen are known to be absorbed by titanium at elevated temperatures. Ehrlichl reports that about 30 at. pct oxygen can be dissolved in solid solution by alpha-titanium. Nitrogen also has a solid solubility in alpha-titanium, but there is no information as to its extent. The solid solubility of hydrogen in titanium also is high. Kirshfeld and Sieverts2 report 50 at. pct soluble, while Hägg3 reports about 33 at. pct hydrogen to be soluble in alpha-titanium. General statements are made in the literature that oxygen, nitrogen, and hydrogen embrittle titanium, but no quantitative measurements have been made of the effect of these gases on the mechanical properties of the metal. One reason for this is the lack of a source of titanium pure enough to be considered a suitable starting material. Iodide-refined titanium, made by thermal decomposition of titanium iodide vapor on an incandescent wire,4 contains small amounts of carbon, silicon, iron, and aluminum, but is very low in oxygen, nitrogen, and hydrogen content, and, therefore, was used in this work. A further reason for the lack of quantitative information on the effect of these gases, particularly oxygen, is the difficulty of carrying out accurate analytical determinations at the low concentrations of interest in this work. For this reason, the oxygen, nitrogen, and hydrogen were added in measured amounts as gases, and diffused into the titanium, to avoid the necessity of chemical analysis. The purpose of the work reported here was to isolate and measure the effects of oxygen, nitrogen, and hydrogen on titanium of the highest purity available at the time. The concentrations studied were 0.25, 0.5, and 1 at. pct in each case. Experimental Work One-half of a 24-in. hairpin of iodide-refined titanium was available for this work. The rod was approximately 0.25-in. in diam and had a 0.003-in.tung sten core. From chemical and spectro-graphic analyses, the purity of the sample was estimated to be between 99.80 and 99.95 wt pct. The chief impurities (aside from the tungsten core) were iron (0.04 pct), silicon (0.01-0.1 pct), aluminum (0.05 pct), carbon (0.03 pct). The tungsten core constituted 0.05 pct by weight of the sample. Although some alloying undoubtedly took place between the tungsten and the titanium during the deposition reaction, the core remained substantially intact in the deposited metal. The initial average hardness of the titanium as deposited was 105 Vickers (10-kg load). The maximum hardness was 116 Vickers and the minimum 91 Vickers. The metal was somewhat harder than that currently being obtained by the iodide process, that is, 75-90 Vickers. The rod was cold swaged to ¼-in. diam and then cold rolled in diamond shaped rolls to about 0.080-in. square, using reductions of 15 pct in area per pass. The 0.080-in.-square wire was cut into 6-in. lengths for the preparation of the alloys by the gaseous absorption and diffusion method. ADDITION OF OXYGEN, NITROGEN, AND HYDROGEN TO TITANIUM A modified Sieverts' absorption apparatus, shown in Fig 1, was used in

Jan 1, 1950

By R. F. Krueger, L. C. Vogel

A design is presented for an electrical analog computer which can solve non-steady state heat transfer problems in an extensive radial forrnation containing a moving cylindrical source. The computer is used to simulate a .simplified thermal oil recovery process in which heat transfer from a moving, constant temperature source takes place radially by conduction only. Temperature distribution curves are .shown for several different assumed modes of travel for the heat source. The data are used to estimate the residual fuel requirements necessary to maintain a self-propagating isotherma1 front for the particular system being studied. Although the computer is designed to represent an unique system. conversion factors can he adjusted to show the effects of changing the assumed values of system constants, such as thermal conductivity of the formation and temperature of the source isotherm. Examples are given to illustrate the relative influence the assumed values of these variab1es will have upon the quantity of fuel required to maintain the source. The maximum effect of heat transfer by the flowing air stream is estimated mathematically, and full requirements for this system are shown to he markedly reduced. Inasmuch as the examples discussrd refer to a simplified process, the results are not directly applicable to a practical field operation. It is believed, however, that the data il1ustr-ate some general trends which are important in thermal recovery processes. Data from laboratory and field experimentation can he used to modify the computer to take into account the influence of heat transfer by various mechanisms, for example, by injected air and by fluids ahead of the hot zone. With .such refinements it would be possible to estimate more accurately the limiting values for the rate of travel of the high temperature front and for the required air- injection rates. Use of this computer should aid in evaluating the economic feasibility of oil recovery by various thermal processes. It is hoped this paper will stimulate further work by others to help accomplish this objective. As the costs of exploration for and development of new oil fields rise. increasing the recovery of oil from established fields becomes more and more important. In fields containing low gravity crude oil, ultimate recoveries by primary means are sometimes less than 10 per cent and often total only 10 to 20 per cent of the oil in place. Conventional secondary recovery methods are not always effective in increasing this total. Methods which have been proposed for increasing the recovery of viscous oils include thermal processes for increasing the mobility of the oil. One method is to provide a moving heat source generated within the formation to heat the oil and a flowing gaseous medium (for example, air) to sweep the oil to the producing wells. The possibility of such a process has intrigued engineers for many years.'. '." but little or no information has been available in the literature relative to the technical or economic feasibility of this method. Recently, however, interest has been revived by publication of laboratory and field test results indicating the feasibility of maintaining

Jan 1, 1956

By Douglas A. Karvonen

INTRODUCTION Although the economy in the Province of Saskatchewan has historically been agriculturally oriented, a major source of wealth has been realized through natural resources such as petroleum and natural gas, coal and uranium and since the 1960's - potash. Potash or potassium chloride, in the form in which it is presently produced in Saskatchewan, is used primarily as fertilizer, a source of potassium, one of three essential elements required for healthy plant growth, with about 5% of production sold to the chemical industry for use in such products as soap and liquid detergent, glass and ceramics, textiles and some pharmaceuticals. Saskatchewan is estimated to have approximately 40% of known world potash reserves and its ten active mines account for some 25% of annual world production. POTASH CORPORATION OF SASKATCHEWAN In an effort to guarantee a fair and lasting economic benefit to the Province of Saskatchewan, the Potash Corporation of Saskatchewan (PCS) was created on February 4, 1975 through an Order-in-Council under the Crown Corporation's Act and later on April 1, 1976, the Potash Corporation Act provided for its continuation. PCS was given the mandate to acquire ownership of a significant portion of the potash mining capacity in Saskatchewan and to establish an organization capable of operating the facilities, marketing the product, and conducting all of the other activities necessary for a successful corporation competing in the world potash industry. The corporation is the largest potash producing and selling organization in the Western World - or third largest in the world. (See also Figure 1). PCS through its wholly-owned subsidiary, PCS Mining, has acquired a whole or partial interest in five geographically distinct producing properties or divisions, representing today more than 40% of Saskatchewan's potash producing capacity. The acquisition of each division was followed by a program designed to exploit and maximize the particular opportunities at each minesite for increased production. To that end, PCS Mining has taken an active lead in expanding to meet future demand and has implemented expansion programs at all properties except for its Esterhazy Division where it has a long-term processing agreement with International Minerals & Chemical Corporation (Canada) Limited. Through its wholly-owned subsidiaries, PCS Mining, PCS Sales and PCS Transport, this provincial crown corporation has the ability to operate as a producer and marketer of Saskatchewan's potash. In certain instances PCS, the parent company, assists in the financing of various projects undertaken by the subsidiaries and in other cases the subsidiary involved arranges its own financing. POTASH RESERVES As a background to the specific issue of financing, it is helpful to describe briefly the nature of the deposit which supports the industry - our collateral, if you like. The potash beds underlying Saskatchewan are sedimentary rock deposits formed by the gradual evaporation of an inland sea during the Middle Devonian period roughly 400 million years ago. Now known as the Prairie Evaporite, this formation stretches from North Dakota and Northeast Montana through Southern Saskatchewan into North-Central Alberta. These beds lie at mining depths ranging from 950 - 1000m (3,000 ft) below the surface, where conventional mining methods can be used, and to 1,650m (5,000 ft), where solution mining must be

Jan 1, 1985

By A. F. Meger

Coal treatment by oil spraying receives special attention at the Georgetown plant for the dividends it pays in satisfying present customers and attracting new markets. Customer satisfaction requires care, quality control, and use of suitable oils. REPRESENTED here are the ideas and varied experiences of many people in the Hanna Coal CO. who have helped develop, over a number of years, an efficient and flexible method for spraying controlled amounts of oil on coal. Since the Georgetown preparation plant began operations early in 1951, oil treatment of coal has received special attention. It is believed that oil treating will satisfy present customers and also attract new markets. The first step in developing the new method of oil spraying was the construction of a dust cabinet for testing 50-lb samples of treated coal with the available oil sprays on the market. Tests results were tabulated for both indoor and outdoor storage. The graph, Fig. 1, shows results of the original tests made with a 700-sec residual blend and a 500-sec lubricating oil on Georgetown stoker coal of 1¼x3/8-in. size.* The advantages of better price, improperly blended can raise havoc. Some.,pale oils also, although odorless when delivered, give off a sweet sickening odor when atomized under pressure. It is recommended that all products be tested before they are used. There is a specific place for all spraying oils. For example, at a power plant a severe dust condition exists around the stockpile area and in parts of the plant. The cheapest spraying oil made, regardless of odor, will do an excellent job in this case and will save the company 3 to 5c per gal or more. Domestic trade, on the other hand, must be carefully handled to prevent complaints about odor, and the only way to do this is to stay with the proved products after the odor tests have been made. The preparation plant at Georgetown has facilities to handle either tank car or tank truck deliveries. Steam is available at the unloading point if the weather is severe, and there is an indicator at the unloading point to prevent overflowing the 20,000-gal underground storage tank. Systematic test samples are removed from each delivery and sent to the lubrication engineer to insure quality control. Fig. 3 illustrates the chutes in which smaller sizes of coal are treated. Fig. 4 shows the entire spraying system. Buried in the ground is a 20,000-gal tank with immersion heaters grouped around the feeder line to insure adequate gravity flow to the pump under all conditions of weather. Oil flows to a 500-gal preheating tank where the temperature is kept about 150°F by six 1½-kw immersion heaters thermostatically controlled. Hot oil is fed through a self-cleaning disc-type filter to the hydraulic pump. Valves and piping make it possible to transfer oil from one tank to another or to drain the lines for maintenance purposes. All this equipment is below ground level in a covered pump room,

Jan 1, 1955

By P. Hudock

Thin films of PbS and CdS have been deposited on insulutiug- sapphire substrates by euzploying a subliwzation technique rising near-equilibriurum conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have mobilities approachitzg values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. By performing the depositiotz of a compound within a small chamber heated to a UNiform temperature within a Vacuum systerrz, it is possible to approach equiilibrium cod-tions r.~litl~irs the chamber. In this way; the sublimation and condensation proceed under near equilibrium co?zditions, and it was found that the properties of dePosited corrzpounds were similar to those of the source material. Oriented PbS films on sapphire have a roor?l- temperature unobility of 700 sq cm per v sec and a T-5/2 temperature dependence characteristic of bulk crrystnls. CdS layers on sapphive Izazse a resistivity ~uhich is corrlpamble to the resistivity of the souvce crystals over a range of four ordem of rrlagnitude. Irz contrast, Ihe resistivity of CdS films prepared by conventional evaporation depends largely upon the substrate terrzperat~ire and postheating treatrrletlt, vather than upon the properties of' the solirce rrraterial. In the case oj the CdS films the achievment of high carrier mobility required the cargful exclusion of cont~~~~ii~unts from the films. The steps taken to accomplish this included presublimation of the source material, performance of the deposition at a backg-m~ozd pressure less than 10-8 Torr, and a solvent extraction with liquid cadminum, similar to that described by Aven and woodbury. The deposition of ,films under near-equilibrium conditions is being op-plied to other classes oj COmpounds. II should he of 1:allce ,tor llle deposition of nny matevial that decomposes in the vapor state. THIN films of PbS and CdS have been deposited on insulating sapphire substrates by employing a sublimation technique using near-equilibrium conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have Hall mobilities approaching values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. Depositions were performed in a small quartz sublimation cell shown in Fig. 1 that contained the compound and the single-crystal sapphire substrate. The substrates were etched in tapered solutions of hot phosphoric acid, rinsed in deionized water, dried, and transferred to the cell under dry nitrogen. Graphite crucibles and substrates were used in experiments where it was necessary to provide an inert test vehicle for the analytical determination of impurities in the source crystals and deposited films. The crucibles and substrates were machined out of spectrographic-grade graphite having less than 1 ppm of impurities. A quartz mask was sometimes used to define a pattern which could be used for Hall and resistivity measurements. Close spacing between the compound and substrate was maintained to insure better transport of each component from the source material.

Jan 1, 1968

By R. J. Wasilewski

The variation of elastic modulus with terrzperature between -150° and 600°C has been investigated. Compounds close to equiatomic cornposition exhibit very low modulus values and very high damping near room temperature. The modulus rises steeply with both decreasing and increasing temperature. The modulus minimum and the high damping are believed to be connected with a martensitic transformation of TiNi. In bulk material this transition takes place slightly above room temperature quite rapidly and reversibly, with a hysteresis of some 30°C, depending on the Ti:Ni ratio. Oxygen impurity affects the reaction time. THE inter metallic compound TiNi has been reported to exist in an ordered CsCl (B2) structure,l-6 the homogeneity range varying rather markedly with temperature.7 Some investigators reported this compound to decompose peritectoidally to Ti2Ni and TiNi, between 650° and 800°C,3 or below,',g the latter workers also suggesting the decomposition to be strain-sensitive. Purdy and Parr were the first to report a structural transformation to a new, possibly hexagonal, structure at 36°C,7 a temperature indubitably too low to allow the significant amount of diffusion necessary for a peritectoid reaction. Mechanical-property investigations of compositions close to TiNi just above room temperature have qualitatively shown remarkable anomalies, particularly with respect to clamping,' and to a "memory" effect, that is, plastically deformed material returning to its original shape on being heated through the "decomposition" temperature.9 The original explanation of this effect—based on the apparent experimental observation of Ti2Ni or TiNi, formation in the material subjected to tensile or compressive stresses, respectivelp—does not appear plausible. It appeared more probable that the change involved may be a martensitic, diffusionless structural transformation, similar to those observed in other B2 structures such as 0 brass,'' AuCd,ll and AuZn.12 The existence of such transformation has been established recently,', although the symmetry of the low-temperature structure is not yet known. The present paper describes the elastic modulus and damping behavior of polycrystalline TiNi in both structures. EXPERIMENTAL METHOD 1) Specimens. All the specimens to be investigated were prepared from premelted electrolytic nickel and iodide titanium by nonconsumable arc melting and casting in a water-cooled copper mold. The cast billets were canned in mild steel, extruded, and swaged to approximately 0.375 in. diam. The cans were then removed by pickling or machining. Preliminary material balance checks indicated no significant weight losses on melting (less than 5 mg on a 50-g button); hence nominal compositions have been used throughout. In agreement with previously reported observations7 no single-phase material was obtained at—or close to—Ti 1.00 Ni1.00 a small amount of finely divided second phase always being present. It was found that most of the oxygen impurity was associated with this minor phase, which was identified as oxygen-bearing Ti2Ni—possibly Ti,Ni,O. The amount of this phase—at any given Ti:Ni composi-

Jan 1, 1965

By M. K. Yen, W. R. Hibbard

Previous studies of plastic deformation of metals have emphasized the important role of bending and constraints during strain under relatively pure stresses.1"5 Some new phenomena such as early conjugate slip6 and polygonization7 are intimately concerned with the relief of bending stresses, the former by slip and the latter by a process analogous to re-crystallization. However, few analyses of the bending deformation of single crystals were found in the literature, and those8,9 are sufficiently previous to the modern interpretations of slip to invite further investigation in this area. The transverse bending mode of testing, using the two-point loading method, was selected because the center portion of the specimen may be considered as under a theoretically pure bending stress with a uniform bending moment. Considerable attention was given to both the lattice distortion and flow characteristics of the crystals during deformation. Experimental Proeedare A specimen under the action of equal and opposite couples at both ends is said to undergo pure bending. The shear and moment diagrams of a specimen under the two-point loading method of transverse bending are shown in Fig 1. The moment over the middle-third of the span is equal to PL/6, and the vertical shear is zero. Fig 2 (A) illustrates the stress distribution in the elastic range on a plane across the middle of the specimen. It can be seen that the normal stress has a maximum value at the extreme surfaces on the tension and compression sides, and decreases proportionately to zero as it approaches the neutral plane. However, when the plastic range is reached, the stress distribution is no longer a straight line relation, but changes in a manner which can be best illustrated as shown in Fig 2(B). The following calculation and stress analysis are mainly in accordance with the works reported by Timoshenkol0 and Kochendörfer.9 From the simple beam formula, the maximum normal stress will occur at the surface of the specimen. For a round specimen with a radius r and for a rectangular specimen with a height 2h and width 2b, the maximum normal stress, Sp, will be given by the following formulas: For round specimen: 2PL Sp = 3pr3 [1] For rectangular specimen: Sn = 8bh2 [2] Since it is reasonable to consider that slip takes place under the same conditions as in uniaxial loading, the resolved shear stress S?, along the operative slip direction will be as follows: For round specimen: 2PL sin x cos ? Sp = 3pr3 sin x cos ? [3] For rectangular specimen: PL S8 = 8bh2 sin x cos ? [4] where X is the angle between the specimen axis and the slip direction and X, the angle between the specimen axis and the major axis of the glide ellipse. It was also reported by Kochenclorfer9 that the critical bending moment, that is, the bending moment exerted on the specimen to initiate slip, should be higher than the value given by the equations stated above. Based

Jan 1, 1950

By J. E. Hilliard

Isobaric sections of the eutectoid region of the iron-carbon phase diagram have been exgerimentally determined at 35, 50, and 65 kb. The phase boundaries were located by metallographic analysis of specimens quenched after equilibriatwn at known temperatures and pressures. With increasing pres -sure a pronounced decrease in the solubility of FesC in austenite was observed together with a depression of the eutectoid temperature. These two effects resulted in a shift of the eutectoid composition toward a lower carbon content; at 65 kb the eutectoid was at less than 0.2 wt pct C. These results are in qualitative agreement with thermodynamic calculations. It has also been shown by calculations that Fe3C in contact with saturated austenite will be stable with respect to both graphite and diamond formation at all pressures above -3.5 kb. 1 HE investigation described in this article was part of a more general study of the effect of high pressure on transformations in Fe-C alloys. Thermodynamic calculations and exploratory runs made in 1959 at the start of the program indicated an appreciable change with pressure in the phase equilibria of Fe-C alloys. However, the calculations were not considered reliable enought to provide the quantitative information required for the interpretation of the effect of pressure on the kinetics of transformations. An experimental investigation was therefore made to determine a series of isobaric sections of the eutectoid region of the phase diagram at pressures up to 65 kb. EXPERIMENTAL PROCEDURE Materials. Seven alloys with analyzed carbon contents of 0.10, 0.20, 0.38, 0.60, 0.77, 0.93, and 1.20 wt pct C were prepared from Ferrovac" iron and high-purity graphite induction melted in magnesia crucibles under argon. The ingots were hot worked and swaged down to 0.19-in.-diam rod which was then centerless ground to a final diameter of 0.125 in. Samples for chemical and spectrographic analyses were taken from each end of the rods. The prin- cipal impurities were found to be Ni, Al, Co, and Si which were present in amounts up to 0.03, 0.02, 0.01, and 0.01 wt pct, respectively. Specimens were prepared by slicing the ground rods into pills 0.06-in. thick which were silver plated to reduce decarburization during the equilibration. Silver was chosen for this purpose because of its very low solubility for carbon and its mutual immisicibility with iron. High-Pressure Apparatus. The high-pressure runs were carried out in the "Belt" apparatus.' As shown in Fig. 1, this consisted of a cylindrical cell compressed between two Carboloy punches loaded by a uniaxle press. Radial support to the cell was given by the "belt" which was a Carboloy die heavily prestressed by a series of steel binding rings. Laminated gaskets of lava and metal separated the punches from the inner surface of the "belt". A cross-section of the high-pressure cell is shown in Fig. 2. Two specimen pills were located inside a resistance heater of 0.20-in.-diam Nichrome tubing. The ends of the tube were sealed with alumina and lava pills tamped in place after the

Jan 1, 1963

By A. B. Dyes, P. H. Braun, B. E. Cole

This paper presents a reservoir engineering analysis of the performance data for a waterflooding project in the Johnson Lease, South Ward field. This type of engineering analysis adds to the knowledge of the mechanics of water flooding. This study reveals that in general (a) high ultimate areal sweep-out efficiencies (95 to 100 per cent) can be expected, and (b) cross-flow among strata of different permeabilities during the fill-up phase can have an important influence on the behavior and should be dealt with in studying reservoirs for water flooding. The analysis further showed that the recovery predictions based on what was considered a consistent interpretation of core data and logs were low because little contribution was assumed from the low permeability, oil-bearing sand sections which have apparently yielded considerable waterflood oil. This project has yielded in excess of 2 1/2 times as much oil by water flooding as by primary depletion. These very favorable results were achieved without the use of any special injection well completion techniques. However, all of the low permeability material war included in the section open to injection despite its poor estimated primary yield. LEASE PERFORMANCE HISTORY The South Ward field lies in the southeast corner of Ward County near the southern tip of the tremendous Yates trend. Deposition of sand bodies along the seashore reefs during the latter part of the Permian period established what have turned out to be ideal conditions to form a great number of independent productive sands. Probably, these reservoirs in Ward and Winkler counties are providing operators with some of the nation's richest sources of secondary oil reserves through the use of waterflooding techniques. In South Ward field water has been very successfully used to flood oil from the Bennett sand occurring at a depth of about 2,300 to 2,400 ft. About 150 ft above the Bennett sand reservoir, the Grand Falls sand produced gas from a large cap extending over most of the field. The Atlantic Refining Co.'s 320-acre W. D. Johnson lease (Fig. 1) is on the northwest edge of the structure with only gas cap apparently present in the Grand Falls sand. The Bennett sand under this lease is oil productive, however, having a gross sand thickness averaging about 80 ft with a net of 18 ft of fairly clean, highly permeable sand, and about 36 ft of oil-bearing sand with low permeability and high water saturation. The lower permeability sand is interbedded with numerous layers of lime, shale, and anhydrite. Radioactivity logs from 12 wells and cores from two, examples of which are shown in Fig. 2, reveal that the total Bennett sand pore volume is about 71,000 bbl/acre. The estimated initial water saturation averages 41 per cent in the 54 ft of sand considered to contain oil; thus, also considering an estimated 18 per cent oil shrinkage, the lease originally contained about 34,000 bbl of oil per acre. Original pressure was probably about 1,400 psig. PVT correlations indicate that the reservoir fluid was originally saturated with gas. After discovery of the field in 1930, Atlantic completed the first well on the Johnson lease in March,

Jan 1, 1958

By R. M. Hudson

The removal of nitrogen from a nitrogenized low-carbon sheet steel that contained 0.011 wt pct N was determined during heat treatment in Hz-N, mixtures. TIze process followed a first-order rate law; that is, plots of the logarithm of nitrogen content in steel were linear with the time of treatment at a given temperature. The rate of removal increased with an increase in temperature from 900" to 1300°F. By 1400°F the rate in dry hydrogen had decreased to a value intermediate between the rates at 1200" and at 1300°F; in wet (2.47 vol pct water vapor) hydrogen the rate at 1400°F was less than the rate at 1300°F and nearly the same as the rate at 1200OF. The rate at a given temperature increased as the 3/2 power of hydrogen concentration in the atmosphere. While wet atmosplzeres were generally more effective than the corresponding dry atmosplzeres, the effect of water vapor was much less pronounced than the influence of hydrogen content. NITROGEN is the principal agent in the strain aging of ferrite, the effect of carbon being secondary.' To eliminate the return of the yield point after straining and aging, it is claimed2 that the amount of nitrogen in solution in steel must be reduced to 0.0002 wt pct. Strong nitride-forming elements (titanium, vanadium, zirconium, and aluminum) can act to eliminate strain aging by combining with nitrogen. It is extremely difficult to decrease the nitrogen content in commercial steels to the low level required by conventional coil annealing because of the poor contact between the strip surface and the reactive atmosphere. However, a variety of gas-metal reactions can be effected by use of the open-coil annealing method,3 in which the metal surface is fully exposed to the atmosphere. With this possibility in mind, the Applied Research Laboratory has studied the influence of time, temperature, and atmosphere composition on the removal of nitrogen from low-carbon sheet steel. MATERIALS AND EXPERIMENTAL WORK Samples from a commercial nitrogenized low-carbon steel (0.010 in. thick) in the cold-reduced condition were used. The chemical composition of this steel is given in Table I. The gas mixtures used are listed in Table 11. The moisture content in the "wet" annealing atmospheres was controlled at a +70°F dew point (2.47 vol pct water vapor) by passing the gas mixture through a glass tube packed with a solid mixture of 10 pct anhydrous oxalic acid and 90 pct oxalic acid dihydrate held at 127°F; this technique has been described previously.4 For "dry" atmospheres, the gas mixtures were passed through a cold trap immersed in liquid nitrogen. A hinged-top Hevi-Duty electric furnace was used with a Vycor-glass furnace tube. When the furnace was at the desired temperature, the gas mixture was passed through the furnace at a flow rate between 1.1 and 1.2 cfh; coupons (size 3 by 3/4 in.) of the steel were pulled into the center of the Vycor-glass

Jan 1, 1964

By J. W. Freeman, D. N. Frey

Fundamental reasons for the improvement in creep resistance of an austenitic alloy by cold working were investigated mainly by X-ray diffraction. The creep resistance was found to be improved by the internal stresses in the lattice of the alloy induced by the cold work. THIS investigation was concerned with the fundamental reasons for improvement in creep resistance of an austenitic alloy as a result of cold working. Also, the investigation was carried out to elucidate the conditions under which cold working could be expected to improve the creep resistance. To achieve these ends, creep resistance and internal structure were correlated for a variety of cold-worked conditions. Since the aim of the investigation was not to obtain specific and extensive information on any one alloy, creep testing was done with a single stress at 1200°F. Structural studies were carried out primarily with X-ray diffraction characteristics. The alloy used, low carbon N-155, was selected on the basis of being representative of at least some of the alloys used in gas turbines. Low carbon N-155 alloy in the form of %-in. sq bar stock was used in this investigation. The chemical composition, in percent, was: C, 0.13; Mn, 1.43; Si, 0.34; Cr, 20.73; Ni, 18.92; Co, 19.65; Mo, 3.05; W, 1.98; Cb, 0.98; N, 0.14; and Fe, balance. The bar stock was produced from a 13-in. sq billet, finished to 7/s in. round cornered square between 2060" and 1910°F. Prior to use in this particular investigation, the bar stock was solution-treated 1 hr at 2200°F and water quenched. This procedure was used in order to put the stock in a condition where effects of prior processing were minimized. Experimental Procedure The specific approach to the problem was twofold. First, the influence of cold working, under various conditions, on the creep rate under a single stress at 1200°F and on the internal structure was in part determined. Second, the effect of annealing at various times and temperatures on the creep rate and internal structure of the cold-worked samples was in part evaluated. The first step was basic to the investigation—creep resistance and structure were to be correlated. The second step was taken to see if the annealed samples showed some internal changes which could also be correlated with changes in creep resistance. This it was felt would facilitate solution of the basic problem. The creep and structural studies were carried out on samples reduced approximately 5, 15, and 40 pct at room temperature and 15 pct at temperatures up to 2200 °F. Annealing of various of the samples was done at 1200°, 1400°, 1600°, and 1800°F for time periods up to 1000 hr. Studies of the annealed samples were concentrated on materials rolled approximately 5, 15, and 40 pct at room temperature and 15 pct at 1400°F. The creep tests were carried out at 1200°F under 40,000 psi, the latter being approximately the 1000 hr rupture stress of the material

Jan 1, 1952

By J. H. Faulk

An examination is made of the various factors influencing drilling rate and drill bit life in various diameter holes. It is concluded that drill bits in the size range 4% to 6 1/4 in. can be used to attain substantially the some daily drilling progress as conventional size bits in soft rock drilling operations. An examination of the most important factors influencing "hazard of losing the hole" in the different hole size results in the conclusion that the smaller hole sizes can probably be drilled at reasonably low risk. However, this risk will be somewhat greater in the smaller diameter holes, requiring that special drilling and mud engineering practices be used to make small diameter holes practicable in soft rock drilling operations. An engineering analysia is made of the power and hydraulic requirements of several drill string-hole combinations to test the feasibility of drilling .small diameter holes in soft rock areas. Large econormies in rig power requirements appear possible by drilling .smaller .size holes in these operations. INTRODUCTION The industry now is re-examining the utility of small diameter holes in the light of substantial technical advances made in recent years. Faced with increasing cost of finding reserves and with proration after developing them, the industry must either develop methods of economizing or receive a lower rate of return on investments. Small diameter holes appear to involve an attractive method of economizing. Our objective is to determine if this is technically possible in soft rock operations. Soft rock, as used in this report, refers to those formations of a "drill-ability" corresponding to that of all Gulf Coast formations shallower than and frequently including much of the Eocene rock system. An important phase of technology which we shall examine is relative drilling rate and bit footage which may be obtained with various size bits. Rig operating efficiency, particularly as influenced by hazard, is also discussed in detail. The technical conclusions resulting from these examinations are used to develop sample drill string design and rig horsepower requirements for drilling holes as smaH as 4 3/4 in. and larger. The principal criterion used for the drill string design is that approximately the same daily drilling progress would be possible in all size holes in soft rock operations. This facilitates a comparison of rig size required for drilling the hole sizes in the range between 4 3/4 and 8 3/4 in. BROAD PROBLEM OF DRILLING RATE AND BIT FOOTAGE The three factors controlling daily drilling progress are: (1) drilling rate of bit while on bottom turning, (2) bit footage, and (3) rig operating efficiency. Let us look now at the first two of these factors. Drilling technology has progressed to the point that a semi-quantitative analysis of the effect of various operating variables upon these factors can be made. Those factors which apparently limit both drilling rate and bit footage for bits now in use are: (1) bit design, (2) weight on bit, (3) hydraulic cleaning capacity for bit cutting surfaces and hole bottom, and (4) rotary speed. (We neglect the effect of mud and formation properties because these factors arc the same for the various size bits.

Jan 1, 1957

By O. D. Gonzalez

ThIS communication presents the results of a determination of the permeabilities of hydrogen and deuterium in a iron from 360° to 560°C. Recently Heu-mann and primas' have given values of the diffusivity and solubility in a iron of the two isotopes from which the permeability can be calculated. The work reported in the present communication, however, is a direct measurement of the rate of permeation of the isotopes through an identical iron specimen under the same conditions, so that systematic errors can be minimized in the calculation of the ratio of the permeabilities—the value which is usually of main importance in establishing limits for isotopic differences in diffusive processes. Experimentally the procedure used was the usual one: a steady-state flow of gas produced by a pressure difference across an iron membrane was observed as the pressure rise with time in a previously evacuated, calibrated volume connected to the outlet side of the membrane, while a constant pressure of gas was maintained on the opposite inlet side. The membrane was a cylindrical tube 9.38 cm long, 0.730 cm inside diam, 0.187 cm wall thickness, fabricated of 99.95 pct vacuum-melted National Research Corp. iron (less than 0.003 pct C). One end was sealed by a heliarc-welded iron (99.95 pctj lid of 0.147 cm thickness; the other end of the tube was welded to a 304 stainless-steel tube (0.318 cm ID and 0.318 cm wall) which connects to a vacuum system and to the calibrated volume including a dibutylphthalate manometer. The temperature of the iron membrane was maintained constant to ±0.l°C and was measured with an iron-constantan thermocouple which was calibrated against a standard Pt/Pt-Rh thermocouple: the temperature variation along the length of the membrane did not exceed ±0.5°C. Hydrogen was allowed to pass through the membrane assembly for 72 hr at 615°C before permeability measurements were begun. The system was tested at temperature before and after the experiments by a substitution of helium for hydrogen in the inlet side; under these conditions the pressure rise observed in the outlet side was negligible at all times. The gases used for the permeability measurements were 99.95 pct Matheson prepurified H2 and 99.7 pct D2 (0.3 pct HD) from the Isomet Corp. The gases were dried with liquid N2 before use. In Fig. 1 the logarithms of observed flows, jt, for a pressure difference of 73.4 cm Hg are plotted against T-1 Each point in Fig. 1 represents the slope determined by a least-square evaluation of a plot of the pressure in the outlet side of the membrane against time, including at least two separate sets of observations. Each point in the figure has an uncertainty of ±0.6 pct arising from the experimental uncertainty in the pressure and time measurements. The standard deviation of the observed pressures from the straight lines in all cases is less than the experimental precision of the measurements. The observed flow, jt, includes a small but not negligible flow through the stainless-steel connection.

Jan 1, 1968

By C. A. Bruch, J. F. Duffey

On the basis of metallographic and cooling-rate studies of 15 U-Zr alloys, a new version of the 6 phase region of the U-Zr phase diagram is proposed. IN several published diagrams of U-Zr alloy system:' there is good agreement that at elevated temperatures complete solid solubility exists between y uranium and ß zirconium. Similarly, there is reasonably good agreement concerning the uranium-rich and zirconium-rich ends of the diagram. However, there is no agreement concerning the nature of the diagram at intermediate compositions and at temperatures below about 650°C. The early work of Saller et al.8 hows an intermediate phase, 6. In a later diagram by Saller and Rough' shown in Fig. 1, the d phase field is drawn with dotted lines, indicating doubt that this phase exists. The diagram of Summers-Smith2 does not show the d phase. More recently Holden and Seymour' have shown that in the composition range 40 to 60 wt pet Zr, the high-temperature ? phase, which is body-cen-tered-cubic, transforms to an ordered structure, 8. They found that the order-disorder transformation occurs between 595° and 610°C, and presented a diagram based on the study of four different alloy compositions. Most recently Saller et a1.5 presented a new diagram which differs with respect to the composition limits of the 8 field from the others proposed by these authors. The purpose of the present investigation was to determine the boundaries of the d phase field. Experimental Procedures and Results Alloys—Buttons, weighing 80 g of 15 different alloy compositions were prepared by arc melting Mal-linckrodt uranium and iodide-process zirconium in a water-cooled crucible. A controlled atmosphere of argon and helium was maintained in the furnace. Prior to making each button, a sacrificial button of zirconium was melted to increase the purity of the furnace atmosphere. Each alloy was then melted six times to improve its homogeneity. Subsequently the alloy buttons were jacketed in copper and hot rolled to slabs at 775°C. From these slabs, specimens were machined for chemical, thermal, and metallographic analyses, Table I gives both the estimated chemical composition of the alloys, and the values which were obtained by analysis. The oxygen contents varied from 0.013 to 0.032 pet, nitrogen from 0.0014 to 0.014 pet, and carbon from 0.0013 to 0.011 pet. The purity of the alloys ranged from 99.947 to 99.975 pet. Thermal Analysis—The specimens for thermal analysis were blocks 11/4 x 1/4 x % in. The bead of a calibrated thermocouple was placed between two of these blocks and molybdenum wire was wrapped around the assembly. Each assembly was sealed in a quartz capsule having an argon atmosphere. The capsule was placed inside a refractory crucible which was heated in a furnace. Using a method described by Smith,' the emf of a differential thermocouple, with junctions inside and outside of the refractory crucible, was used to activate the

Jan 1, 1959

By E. Marburg

Most ingots complete solidification vertically rather than transversely. This conclusion is based on complete solidification patterns of big-end-up and big-end-down ingots developed from dumped and split ingots. New mechanisms for segregation in ingots are proposed. Internal soundness in ingots is found to depend upon adequate width of vertical core. A LTHOUGH it has long been recognized that the A internal soundness of ingots is principally been recognizedthatthedependent on the process of solidification, knowledge of this process is still only fragmentary. The mechanisms causing the several types of segregation in ingots, which mechanisms are necessarily related to the solidification process, are not well understood. In absence of a better conception of the solidification process, it seems hardly surprising that mold design varies widely. Guiding principles for mold design are needed. At stake in the improvement of ingot quality are not only improved properties of steel but also appreciably higher yields of sound steel, which would considerably decrease manufacturing costs. In the present study, following a general description of the several types of segregation in ingots, Fig. 1, complete solidification patterns of a big-endup and a big-end-down ingot, including the zones of accelerated solidification, have been reconstructed. In both ingots, a core of vertical solidification extends from the base cone to the hot-top junction. Based on the finding that ingots complete solidification vertically rather than transversely, as has been previously assumed, new mechanisms for segregation in ingots are proposed. Internal soundness in ingots is found to depend upon the width of the vertical core, which in turn depends principally upon the width to height (w/h) ratio of the ingot. Solidification patterns of ingots are of three general types: 1—those in which vertical solidification does not reach the top, 2—those in which vertical solidification just reaches the top of the ingot, and 3—those in which vertical solidification reaches the top some time before transverse solidification would reach the middle of the ingot, so that a vertical core of definite width at the top of the ingot is developed. Axial defects vary characteristically with the solidification pattern. Examples of ingots of each type are presented. Dumped ingot data reported by Nelson' have been used in developing families of curves of transverse and vertical solidification, and in deriving the effect of the w/h ratio upon the solidification pattern. Photographs of many ingots split at Homestead and at Duquesne Works, United States Steel CO., as well as those published by the British Iron and Steel Institute,' have been studied and analyzed. In the interest of brevity, only typical ingots of each type or classification from the above sources have been reproduced. Segregation in Ingots Segregation in ingots falls into three principal classifications: 1—lamellar segregation, as revealed in sulphur prints (Figs. 2 and 3); 2—zone segregation, or broad variations in composition; and 3— interdendritic, or microsegregation. The last class, of minor importance, is not considered here. When liquid metal cools, according to the theory of differential or selective solidification,2 metal of relatively high purity selectively solidifies first. Liquid segregates (principally carbon, phosphorus,

Jan 1, 1954

By W. C. Winegard, E. L. Holmes

The effects of the solute elements lead and bismuth on grain growth in zone -refined tin have been investigated. At low temperatures, viz. below 160°C. or at high concentrations, viz. greater than 0.03 at. pct, the temperature dependence of grain growth was found to be constant. A correlation was found to exist between the rates of grain growth in the presence of solute impurities and the factor [C Ir - 1]2 , where C is the solute concentration, r is the radius of solvent atom, and r' is radius of solute atom. It is shown that the Liicke and Detert theory does not give a satisfactory explanation of the results obtained. INVESTIGATIONS of grain growth in zone-refined lead and tin and some effects of solute elements on grain growth in these metals have been reported by Bolling and winegardly2 and Holmes and winegard? The present investigation is an extension of the previous work, and was undertaken to provide additional results which might make it possible to discover the mechanism whereby the rate of grain growth is affected by the presence of foreign solute atoms. The experimental procedure was exactly the same as that described previously.3'4 Figs. 1 and 2 show the results obtained with lead and bismuth additions over the same temperature range, viz. 167" to 220°C, as that used for the investigation of grain growth in zone-refined tin.3 Fig. 3 shows the results obtained for zone-refined tin and for this tin with lead solute additions over an extended temperature range. DISCUSSION OF RESULTS As mentioned previously,3 the character of grain growth in the particular zone-refined tin used in these experiments appears to change as the temperature of annealing falls below about 160°C. The grain growth became somewhat irregular and was characterized by a jaggedness of many of the grain boundaries. The reason for this change is not known, but may be due either to residual impurity effects or possibly an oxide precipitation. It was obvious that normal grain growth only occurred in the zone-refined tin through the high-temperature range 167" to 220°C, and so the effects of solute atoms on grai11 growth over the two temperature ranges will be discussed separately. a) Effect of Impurity on Grain Growth in the Temperature :Range Above 167°C. It is apparent from Figs. 1 and 2 that, for low concentrations of solute, the rates of grain growth tend towards a common value as the melting temperature of tin is approached. As the concentration of lead is increased, the rate of grain growth close to the melting temperature is also reduced, and at high concentrations the temperature dependence of the rate of grain growth appears approximately constant. It should be noteil that the effect of bismuth is greater than that of the same concentration of lead, but both these solutes have a smaller effect on the rate of grain growth than silver, as seen from an earlier investigation of Holmes and Winegard. It should

Jan 1, 1962