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Jan 1, 1967

Organization Place Date 1919 American Chemical Society :.... Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters' Society, First Annual Convention Chicago, Ill. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, 0. Sept. 29-Oct. 2

Jan 7, 1919

Organization Place Date 1919 American Chemical Society Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters' Society, First Annual Convention Chicago Ill. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, O. Sept. 29-Oct. 2

Jan 8, 1919

By Ivan B. Cutler, Milton E. Wadsworth

Coprecipitation of anionic and cationic polyelectrolytes has been applied to floccula-tion of several mineral systems. Results obtained in a study of the flocculation of kaolinite and hematite suspensions of polycationic and polyanionic electrolytes are presented. Greatly increased settling rates were observed following precipitation of positive and negative polyelectrolytes on the surface of finely divided minerals in aqueous suspension. The ratios of polycationic to polyanionic electrolytes required to produce maximum sedimentation have been shown to correspond closely with the equivalence points obtained by light scattering studies of systems containing the positive and negative polyelectrolytes by themselves. DISPERSION of colloids has been of interest to surface chemists for many years. Flocculation studies have been employed to evaluate the limits of colloid stability. In water suspensions, colloids become unstable and flocculate when the 5 potential, the potential of the kinetic solvation sheath, falls to a value at which van der Waals forces may act to draw the particles together. This may happen through an adjustment of the pH of the suspension or by addition of a salt. Optimum conditions for rapid formation of large flocs are found in the region of minimum < potential. In addition to these well known considerations, colloids in water suspensions are known to be flocculated by certain large organic macromolecules. These polyelectrolytes in some cases minimize the 5 potential and in other instances increase the attractive forces by supplying sites for hydrogen bonding.&apos; Use of organic polyelectrolytes in flocculation of mineral colloids has increased rapidly in recent years. These materials are now recognized as indispensable aids to fluid-solid separations in many extractive metallurgical operations. They have been found to increase both the settling rate in thickeners and the filtration rate of filters. In the elucidation of the characteristics of these organic reagents as floc-culants in this laboratory, it was discovered that interaction of certain polyelectrolytes had a surprisingly good effect on flocculation of mineral colloids. Experimental Procedure: The anionic flocculants used in this study were Lytron 886 and 887, produced by Monsanto Chemical Co. Both reagents are copolymers of vinyl acetate and maleic anhydride. Lime is added to Lytron 886, whereas Lytron 887 is all organic. These reagents possess two carboxyl groups for each acetate group and are therefore anionic in character. The cationic reagents used were the Peter Cooper Co. 1-X and 2-X glues. The structures are not definitely known, but the re- agents are amines and are cationic in character. The glues were prepared in the chrome-alum form. Both types of reagents may be classified as polyelectrolytes in that they are high molecular weight polymers and ionize in water. All data presented are in terms of sedimentation rate, measured in 250-ml glass-stoppered graduated cylinders. With suitable precautions such measurements are fairly reproducible and provide a sensitive means for selecting important parameters such as PH, reagent concentration, and floc size and density. Agitation was standardized with five complete end over end cycles of the suspensions in the stoppered graduated cylinders.

Jan 1, 1957

By H. T. Kennedy, S. G. Dardaganian, J. L. Clanton

This paper presents equilibrium ratios measured on oil and gas samples taken from the Kelly-Snyder field at the reservoir temperature of 128°F. From these data smoothed curves were constructed for the reservoir fluid up to the bubble-point, 1,874 psia. A material balance calculation, based on the use of equilibrium ratios instead of the usual solubility and shrinkage meayr~rements is made on the field and compared to the con\.entional method. DETERMINATION OF EQUILIBRIUM RATIOS The equilibrium ratios, or K values were obtained by recombining separator samples of oil and gas taken when the reservoir was above its bubble point, and thus represented the reservoir fluid before any change had occurred due to the evolution of gas. The well sampled had a gas-oil ratio of 617 cu ft of high pressure sepalator gas per barrel of separator oil. and a bottom-hole temperature of 128°F. Samples were brought to equilibrium by agitating for 24 hours in a thermostat, maintained at the proper temperature within 0.2ºF, mercury being added when necessary to maintain the pressure constant. Samples of oil and gas were then taken by constant pressure displacement, and analyzed by low temperature frac-tionation. Equilibrium ratios were determined at 128°F and 500, 800, 1,000 and 1,400 psig. At the latter pressure, there were indications that the gas samples were contaminated with small quantities of oil, and only data taken at the first three pressures were included in Fig. I. This figure has been extended to higher and lower pressures by the use of the Fluor charts for 3,000 psi convergence pressure, on which the experimental points fit well. MATERIAL BALANCE EQUATIONS The possible errors involved in conventional material balance equations have been analyzed by Muskat1. Where the errors occur in field measurements, or in obtaining effective averages from variables such as gas-oil ratio and pressure, they will evidently be involved in any attempt to estimate the content of the reservoir. On the other hand, substantial errors may be introduced in conventional material balance calculations by: (1) the neglect of the amount of oil dissolved in gas at high pressures and temperatures in the reservoir, but which condenses under separator conditions; (2) the assumption that the separation of oil and gas in the reservoir may be duplicated by a differential liberation in the

The income of the Institute is derived from dues, subscriptions to MINING AND METALLURGY and sale of publications. These sources are fortunately supplemented by the interest from invested funds now amounting to over $500,000, a considerable portion constituting endowments for especial purposes. Aside from the medal funds the principal endowments are the James Douglas Fund for support of the Library, the Rocky Mountain Fund and the Seeley W. Mudd Memorial Fund. The income from the two last named is available for the support of research and a variety of other purposes. It is allocated by the Board of Directors upon recommendation of standing committees in each case. An active effort is being made to increase the endowments of the Institute, it being felt that unusual opportunities exist for research and public and professional service through the organization.

Jan 1, 1936

By F. W. Bowdish

Analysis of data on the equilibrium exchange of sodium ions from salt solutions for calcium ions, from various fractions of an oxidized calcareous iron ore from Lorraine, France, strongly suggests that the calcium may be attached to the solid by only one of its bonds. Nearly equal values were found for the equilibrium expression from data covering concentration ranges of 1000 fold for the salt and 235 fold for the ion-exchangeable calcium. Differences indicated between the exchangeable calcium contents of the slime and the sandy portions of the ore, as well as the equilibrium relationship itself, are of importance in the flotation of the ore. During an experimental program on the flotation of oxidized calcareous iron ores from Lorraine, France, ion-exchangeable calcium was found in the ore. Because this source of calcium ions, if not controlled, could thwart all efforts at flotation, an extensive study was made of the phenomenon. The part of that study reported here was to obtain data on the equilibrium established between ore solids and solutions of sodium chloride, and to analyze the data to try to understand better the physical chemistry of the exchange. The ore contains oolites of goethite and quartz grains embedded in a matrix consisting of calcite and a brown cement believed to be the residue from oxidation of the silicate minerals found in fresh unoxidized ore. When ground, a substantial fraction of the ore becomes a fine slime in which is concentrated more than half of the alumina content of the ore. It is believed that the alumina occurs as unidentified clay minerals with which most of the ion-exchange capacity of the ore is associated. A preliminary experiment on the exchange of ions from the ore for sodium ions from solutions of NaCl showed that calcium was about ten times as abundant as magnesium in the exchange solutions. Thus calcium was the predominant ion in causing difficulties with flotation, and it was the only one for which data was obtained in this study. It is believed that the omission of magnesium ion exchange from consideration does not invalidate the results. It is possible, however, that inclusion of magnesium in the analyses and calculations or its prior elimination from the samples would have improved the consistency of the results. EXPERIMENTAL Data about the equilibrium exchange of sodium from solutions for calcium from the solids were obtained using two different samples of material. The solids

Jan 1, 1963

By H. P. Willard, R. W. Gates

Basic Inc., has been mining magnesite and brucite for 27 years at Gabbs, Nev. This is a medium sized open-pit mine. The magnesite deposits are in north-western Nye County about 30 miles east of Luning, Nev., on the west slope of the Paradise Range, at an elevation between 5000 and 6000 ft. The magnesite and associated brucite is used to make magnesia refractories employed principally in the steel industry and magnesium oxide for various chemical uses.

Jan 10, 1963

By S. R. B. Cooke, H. S. Choi, I. Iwasaki

In a previous article1 the function of various fatty acids as collectors for iron ores was reported for the two alternate processes; (a) the flotation of iron-oxide minerals, and (b) the flotation of calcium-activated siliceous gangue. The selectivity of separation was shown to be markedly dependent not only on such common parameters as pH and the levels of collector and activator addition, but also on the structure and the degree of unsaturation of the acids used. The iron ores employed consisted primarily of hematite, goethite, and quartz and as the effectiveness of any one acid on the separation depends on the individual response of each constituent mineral toward the given collector, a comprehensive knowledge of the floatability of the individual minerals is desirable for the interpretation of the results obtained. The mechanism by which a collector ion becomes attached to a mineral-solution interface has been a subject of much investigation. From quantitative studies of the properties of the electrical double layer on mercury2 and on several solid surfaces3,4,5,6 , the adsorption of some flotation reagents at the mineral-solution interface is beginning to be understood. For example, it has been demonstrated from streaming potential measurements made on quartz5 and corundum6 that the interfacial electrical condition is strongly dependent on the pH. Thisoccurs presumably through the following electrolytic reaction at the interface, and in the presence of a flotation collector, controls the floatability of the solids. A concurrent investigation of the flotation behavior of goethite and of quartz carried out at the School of Mines and Metallurgy7 has shown a positive correlation with the electrokinetic behavior of these minerals. The purpose of the present investigation was to collect general information on the floatability of hematite, and to investigate the function of various 18-carbon aliphatic acids on the floatability of hematite, goethite, and of activated quartz. Electrophoretic mobility measurements, simplified flotation tests using a modified Hallimond tube, and contact angle and frothability measurements were employed. The results are of direct application in the interpretation of the batch flotation results on natural ores as

Jan 1, 1961

By John Ward Smith

Dawsonite-bearing oil shale of Colorado&apos;s Green River formation offers a unique and vast (more than 5.9 Gt of A120 j) resource of easily extractable alumina. The processing methods required by the thermal reactions of dawsonite and its oil-shale carrier also require production of shale oil, soda ash, and nahcolite as marketable coproducts. These production methods are presented. The alumina production process is contrasted with the Bayer process to describe technical advantages of extraction of alumina from oil shale which may offset the problems associated with processing a relatively lean ore. While alumina production from oil shale requires development of new technology, the technical problems appear solvable. Only the political problems arising from the now onerous and completely unnecessary federal oil-shale withdrawal appear less solvable.

Jan 1, 1982

By AIME AIME

THE Iron and Steel and Institute of Metals Divisions will meet jointly at the Statler Hotel, Detroit, Oct. 4 and 5, during the Metal Congress, Oct. 2-6. The Wire Association, the American Welding Society and the American Society for Steel Treating, together with the two Divisions of the Institute, constitute the Congress this year, and each body offers an interesting technical program. The National Metal Exposition will, as usual, be held concurrently. Visiting metallurgists will find themselves engaged in a bit of research not listed in the program-a time study of how best to exploit in a few days both the Congress and all that the place of meeting has to offer. For Detroit, the beautiful "City of the Straits," is third in rank industrially in the United States, and its great manufacturing plants offer much of metallurgical interest. This is especially true of the automobile plants which will be open to members of the various societies during the week of the Congress.

Jan 1, 1933

By Ling Yang, John Henderson

Self-diffusion coefficients of copper in molten copper have been measured by the capillary reservoir method in the temperature range 1140o to 1260°C. The results can be represented by the equation D = [(1.46 * 0.01) x 10-3) exp [(-9710 * 710)/RT] cm2/sec. The energy of activation agrees within the limit of experimental uncertainty with that for viscous flow. The relationship between the diffusivity and coefficient of viscosity is best described by the equation D = kT/4pnr cm2/sec. MEASUREMENT was made of the self-diffusion coefficient of copper in molten copper in the temperature range 1413º to 1533ºK, using the capillary reservoir technique and CU64 as the radioactive tracer.The procedures for filling the capillaries, making the diffusion run and evaluating Dcu from the counting results were the same as described previously.1,2 All experimental operations involving the melt were carried out in a purified argon atmosphere. A graphite crucible, enclosed in a McDanel tube, was used as a container for the melt because of its satisfactory nature as a refractory material and the low solubility of carbon in copper. Graphite was also used for the capillary material. A McDanel thermocouple sheath, to which graphite radiation shields were affixed, was used to hold the capillaries. By moving this sheath through a rubber seal at the top of the McDanel tube, the capillaries could be lowered into or raised out of the melt. A Globar furnace with a constant temperature zone (± 2°C) of 2 in. was used to heat the assembly. The temperature of the furnace was the equilibrium value corresponding to a given setting of the transformer. Temperature was measured with a Pt-10 pct Rh/Pt thermocouple and varied during a run

Jan 1, 1962

By L. M. Kaas

Production planning techniques, particularly a production scheduling model are proposed for use in taconite mining in Minnesota. Applications of the scheduling model, on a two-year mine plan, which evaluates the equipment involved, are detailed. Data and tables are included. INTRODUCTION Fifty years ago Walter Swart, a mining engineer investigating the Minnesota taconites for the Jackling interests, made this report: "There is no doubt in my mind that this taconite mining is a game worth playing and that it can be played to a successful finish. It seems now only a question of men, money, methods and details."&apos; The prosperous industry envisioned by Swart and other taconite pioneers is today a reality. Its growth has been spurred by technological advances in mining and beneficiation, depletion of natural ore reserves, and improvement of the economic climate. However, the massive problems that were solved to make this development possible are only a foreshadowing of the questions of "men, money, methods and details" that will be encountered in the future. The increasing demands for higher quality taconite pellets have already forced producers to examine better methods of quality control for their operations. THE NEED FOR PRODUCTION SCHEDULING The maintenance of fairly constant crude ore characteristics is of major importance to mill quality control. Through careful mixing of ore from storage bins, the concentrator staff can partially reduce the deviations of the feed analysis from the analysis desired. However, the limited effectiveness of bin mixing systems has caused some mining companies to utilize large capacity blending piles to reduce grade variations. Although the analysis of material being reclaimed from such a pile is relatively uniform, raw materials still must be scheduled from the mine into the pile in such a manner that the average analysis of all material is close to the feed analysis prescribed by the mill. PRODUCTION SCHEDULING MODEL Minnesota taconite mining companies have used three analyses to estimate how a certain ore will react to concentration. These factors are the crude magnetic iron content of the ore, the iron content of the plant concentrate produced from the ore at a standard grind, and the grindability index of the ore. The actual laboratory tests used to determine these factors have been described by Apuli.2 These data are obtained from analysis of diamond drill cores, and are the established criteria used by mine planning engineers to formulate taconite production schedules. Variations in the grade of mine output should be controlled by any production scheduling system. However, to be truly practical, production scheduling methods must also consider many of the less tangible variables that affect mine operation. These include pit layout, available equipment, and ownership of ore leases. The number and scope of the variables inherent in this type of mine planning suggested that a computer simulation could be used to solve the problem. The preparation of information for use with a computer simulation program was the initial phase of this project. Meaningful data was developed from logs of diamond drill cores. Analyses were related to their respective areas of influence by means of mine maps, Fig. 1. The three assay variables and tonnages for each area were punched on cards. In addition to these values, a location code number was punched in the first eight columns of the cards. This code is explained as follows: Column 1 Bench number Column 2 Quadrant location as determined by mine reference lines Columns 3-5 East-west coordinate Columns 6-8 North-south coordinate The heart of any simulation techniques is a well engineered mathematical model. To develop a model for taconite production scheduling, the relationship between the three assay variables had to be established. Because changes in each analysis factor affect the mill circuits in different manners, a weighting system was used to determine the relative im-

Jan 1, 1967

Organization Place Date 1919 American Chemical Society Philadelphia, Pa. Sept. 2-6 National Assn. of Stationary Engineers Huntington, W. Va. Sept. 8 American Peat Society Minneapolis, Minn. Sept. 22-24 American Iron, Steel Electrical Engineers St. Louis, Mo. Sept. 22-26 American Institute of Min. and Met. Engineers. Chicago, Ill. Sept. 22-27 American Steel Treaters&apos; Society, First Annual Convention Chicago, 111. Sept. 22-27 National Exposition of Chemical Industries.... Chicago, Ill. Sept. 22-27 National Safety Council Cleveland, O. Sept. 29-Oct: 2 American Foundrymen&apos;s Association Philadelphia, Pa. Sept. 29-Oct. 4

Jan 9, 1919

By L. D. Keller

The application of hydraulic concentration to large scale operations has been effectively accomplished by the use of the SiphonSizer. Operation has been simple, automatic and essentially trouble free. The use of the primary desliming SiphonSizer on magnetic taconites has shown an improvement in grade of concentrate and an increase in recovery over conventional hydroseparators. Magnetic concentrates have been further deslimed and upgraded in SiphonSizers by floating a coarse middling product away from the heavier concentrate. The application of the Siphon-sizer to closed circuit grinding has met with only partial success to date. Hydraulic concentration of minerals has been practiced for a good many years. Until recently, however, the practice has been limited to equipment using a multiplicity of small pockets and relatively low tonnages and flows. The adaptation of the SiphonSizer to the concentration and classification of magnetite has changed this concept. Some fifty commercial units varying in size from a 16-ft diam circular unit to a 25x100-ft rectangular unit are currently in operation on magnetic taconites. Additional units up to 38 ft diam are under construction. Depending upon the application in the flowsheet, upgrading varies from 0.75% to 14% Fe in a single stage. To those not familiar with taconite processing, the importance of the struggle to remove economically as much silica as possible may not be fully appreciated. Perhaps some figures pertaining to transportation costs will underscore this important process. If the silica content of the concentrate from a 10,000,000 ton per year plant could be reduced by I%, a savings in boat freight, at $2.00 per ton, would amount to $200,000 annually! THE SlPHONSlZER The SiphonSizer, as illustrated in Figs. lA, 1B and 2, is a hydraulic classifier in which the hydraulic water is distributed uniformly across the bottom of the vessel by means of a system of headers (1 and 2), jet pipes (3), and nozzles (4). The depth of the teeter bed is automatically maintained by the siphon-float assembly. The feed is introduced through a feed well (5) and separated into two fractions by the effects of rising water and the density of the teetered bed. The magnetite fraction is discharged by the siphon (12) while the fine slime and light middling overflow a peripheral weir (9) to the overflow launder (6). The bed depth is controlled automatically by float valves (7), which are responsive to changes in the height of clear water supported in the superelevation tubes (8) by the density of the teetered bed. On top of the float (7) is a needle valve (10) which permits

Jan 1, 1963

By A. Thielen

In experiments for the production of steel the principal problem has always been the introduction into, or removal from, the iron of a definite quantity of carbon. Although the solution of this problem had engaged a more or less blindly and empirically directed effort for a long time, it was only with the development of analytical chemistry that the rôle which carbon plays in the constitution of steel was disclosed in its full significance, and that many of the problems confronting the steel-maker were thereby more clearly defined than before. For a long time, and to a certain extent even to this day, the percentage of carbon in steel has been the controlling means of deter mining its quality and hardness. In many cases the percentage of carbon alone has been relied on for judging large consignments, such as the large deliveries of wire-billets and blooms to America during the past twenty years; and though to-day the influences of the other constituents are recognized and many other considerations are taken into account, and though, moreover, some special steels, such as the Hadfield manganese steel, apparently dispense to a certain extent with the assistance of the carbon, yet fix our Bessemer, Thomas, Siemens and crucible steel the carbon still remains one of the most important constituents, and I venture to say it is indispensable. In order to produce in the Bessemer converter a steel of a certain required percentage of carbon, two methods, as is well known, present themselves. By the one the decarburization process is stopped when the desired carbon limit in the bath has been reached ; by the other the bath is completely decarburizecl, and then a calculated amount of carbon added in the form of spiegel, ferro manganese, etc. In Germany the latter method only was adopted, and it was retained when the Thomas-Gilchrist process for the production of low-Phosphorus steel from high-phosphorus iron eame into use, since from the nature of the new process complete decarburization is neces-

Jan 1, 1891

Jan 1, 1967

By W. Hurst

The authors of this paper, in substituting values in a material balance equation associated with a gas reserve and a water drive, cannot find sustainment of what the gas in place should be; therefore, their conclusion is that this type of problem dealing with gas reservoirs is insoluble. They have introduced the word, "cybernetics," based on the work of Norbert Wiener, that further extends this line of reasoning, namely, to the effect that the system is a "black box", and that the gas reservoir and aquifer can take on infinite aspects &apos;based upon their past performance, to quote the authors. The inference is that this black box is an unknown. which permits in computer programming to subscribe as many variables as possible to observe by adjustment of one to another those combinations of conditions that fit field behavior. This may satisfy those in this discipline whose dedication is to programming, but to the others this is a comparison to the rationalization of the combinational results of the throwing of dice—a probability procedure. In reservoir engineering we are more direct. We learn from the examination of individual we&apos;ll and field data exactly what is in this black box. I now come to the impasse that has confronted these authors in their machine calculations. In this I have reproduced from their own production data (Tables 1 and 2 of their paper) pressure vs cumulative gas produced. shown as Figs. D-1 through D-5. A perusal of any of these five plots, for the corresponding fields in the Po Valley, shows the straight-line relation of pressure vs gas produced, evidencing pressure depletion. The point I make is that in their fundamental production data, there is no variance from a straight line that can support a water drive.

By Enrique Touceda

FOR a number of years prior to the world war, the firm of Geo. H. Thacher & Co., of Albany, N. Y., was engaged in the manufacture of marine and other gray-iron castings. At -the outbreak of the war the firm decided to specialize in the manufacture f propeller wheels. It attacked the problem, therefore, from a foundry point of view, seeking to produce a casting that would be so accurate that no subsequent machining would be required on the blades, also from the point of view of the ship builder. There were two general methods f manufacture, the shortcomings of which have been freely acknowledged. In the sweep method, the nowel, or bottom half-mold, for each blade is swept up by a spindle beam and pitch race, while the top half-mold for each blade is built up individually. In the pattern method one individual blade, with the hub or hub portion, is mounted on a spindle and the individual -blade mold formed, the pattern is then rotated on the spindle to the position- for the next blade, etc. In rare cases wheels were made from a solid pattern. Owing to the cost of the pattern, its failure in many instances to be correctly made, and (when made of wood) its early and sure distortion the disadvantage of this practice is obvious, while metal patterns in most instances were prohibitive in cost. In these methods both green-sand and loam molding was practiced. The casting produced by either method can be considered only as a blank from which the propeller must be machined. The back surface f each blade must be chipped too the templet and through this procedure chipped to such accuracy, as will be required for a static balance. Inasmuch as the&apos; work done by the machine tool is confined to the driving face of the blades, not only is perfection most difficult, but corrosion will be greater because of the removal of the dense skin f the casting and the local strains set up by the pneumatic tool in chipping. To produce a finished 9-ft. propeller for a Navy destroyer required from 8 to 21 days f foundry work and about the same length of, time for the machining. Through the use f the Thacher process, only as many hours are required, besides it is possible to produce a finished casting in perfect conformity, with any particular propeller-wheel design,

Jan 4, 1921

By B. A. Kulp, R. R. Reeber

Lattice parameters for the wurtzite form of&apos; CdS mere measured by powder X-ray diffraction techniques over the temperature range 26° to 1000 K&apos;. A negative thermal -expansion coefficient was determined parallel and perpendicular to the c axis below 13.5°K. Near 808°K, the curves of the a, parameter, the differential thermal expansion, and the resistivitv vs absolute temperature exhibited a reversible discontinuity. j\. direct determination of the lattice parameters of CdS over an extended temperature range is of particular use in interpretation of the effects of high pressure on the band structure of semiconductor materials. For example, Langer&apos; has studied the effects of pressure on the absorption edge of CdS from 77°K to room temperature. In order to properly interpret his results it is necessary to know the change in lattice constants as a function of temperature for the wurtzite, zincblende, and rocksalt2 modifications of this material. Thermal-expansion measurements for CdS, wurtzite phase, have previously been determined over a limited temperature range.s74&apos;5 The zincblende phases, of other compounds with similar bonding, have been investigated by Novikova et a! .&apos;&apos; Previous thermal-expansion measurements for metals with hexagonal symmetry have for the most part used bulk sample techniques for low-temperature result. Most X-ray measurements at low temperature have been on materials with cubic symmetry.&apos;jQ The use of X-ray powder-diffraction techniques offers a convenient and accurate method of measurement over a wide temperature range. The X-ray method, besides measuring unit cell size, also provides information about change in structure type and the nature of some of the stacking defects present. I) EXPERIMENTAL PROCEDURE The thermal expansion was measured by X-ray powder-diffraction techniques. Lattice parameters for the range 300" to 1000°K were determined in a 19-cm Unicam camera. From 26" to 300°K a 34-cm back-reflection camera with the Van Arkel" film arrangement was used. The sample was bonded to a copper cold finger below a helium, hydrogen, nitrogen, oxygen, dry ice, or ice brine bath in a metal cryistat. che inner bath was surrounded by another one for radiation shielding. Nitrogen was used in this outer bath for the very low-temperature runs while dry ice and acetone was used for the 195°K point. CuKa X-rays, filtered with a nickel foil, entered the cryostat through a 0.001-in.-thick aluminum window. During a typical 9-hr exposure the sample was continuously rotated through a 30-deg arc. Heat losses from the sample holder limited the minimum temperature attained to 26°K with helium in the inner dewar. Temperature calibration between 25" and 125°K was determined with an Allen Bradley 300-ohm carbon resistor. The resistor was attached to the back of the copper finger with a thin layer of silicone grease. Liquid He, HZ, N2, and O2 baths were used to calibrate the resistor. Temperature variation is estimated to be *2"K with a slightly higher uncertainty at room temperature and 264°K. The thermal expansion of high-purity germanium from 373" to 900°K was measured as a calibration for the Unicam camera. This value was compared with the known value1&apos; for the thermal expansion. A discontinuity in the thermal-expansion coefficient of the CdS a, parameter was observed. Similar discontinuities in the resistivity and differential thermal analysis at the same absolute temperature indicate that the temperature error is *5°K in the temperature range above 500°K. Temperature errors in the Unicam camera below 500°K are appreciably higher due to large gradients in the resistance furnace. II) SAMPLE PREPARATION The CdS was Eagle Picher ultrapure grade. The crystallite size range of the as-received powder

Jan 1, 1965