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By H. E. Lee, P. C. Feddersen

Greenockite is the only known cadmium mineral of importance. It occurs rather universally, in minor concentrations, as a secondary mineral in sphalerite deposits. The world's cadmium output is obtained through the processing of metallurgical by-products, largely from the treatment of residues from electrolytic zinc, retort zinc and lithopone plants. These sources are supplemented by the processing of fumes from lead and copper smelting operations. The development of modern selective flotation practice in the decade 1920-1930, which permitted the economical mining of complex lead-zinc ores, resulted in significant increases in the quantities of cadmium entering lead smelting systems. Being closely related to zinc as to occurrence, properties and production, most detailed description of cadmium recovery methods are to be found recorded in connection with zinc metallurgy. Other than occasional articles pertaining to particular operational procedures, literature offers but little in the nature of a balanced survey of lead smelter cadmium recovery practices. While many of the basic operations described for the recovery of cadmium from zinc by-products are applicable to the treatment of lead plant products, the inherent problems involved differ widely. In general the cadmium content of related by-products from routine lead smelting operations is present in lower concentrations, exists in a less soluble state and is associated with both a greater quantity and a greater variety of detrimental impurities. To cope with these problems, lead smelter practices are found to follow the general outline: Preparatory Processing 1. Concentration operations 2. Sulphation operations Cadmium Plant Processing 1. Leaching operations 2. Purification operations 3. Sponge precipitation operations 4. Metal recovery operations 5. Refining and casting operations As in the case of related zinc plant operations, cadmium recovery practices at lead smelters are not standardized. They not only vary as to type, but also extent. Depending upon prevailing conditions, lead smelter cadmium operations range from simple concentration campaigns, for the purpose of sufficiently "up-grading" products for shipment elsewhere, to complete processing steps for the production of refined metal. Preparatory Processing The cadmium content of lead smelter receipts is low and, as a rule, proportionate to the zinc content; the usual range of cadmium contained being of the order of 0.01-0.05 pct. Were it not for the low boiling point of cadmium, such small concentrations would, no doubt, be lost in the large tonnages of slag, metal and other smelter end products. However, the ready volatility of cadmium and its compounds at prevailing lead smelting temperatures results in its concentration in fractional portions of fume collected. This collected fume comprises a circulating load within the smelter system. Thus, the cadmium content of blast furnace fume* increases with each successive circulation until an equilibrium value is reached when the sum of the cadmium losses, due to handling and in slag, waste gases and other end products, becomes equal to the intake as ore. With ore receipts averaging, say 0.03 pct cadmium, the concentration value obtainable, through fume circulation in a routine manner, approaches 10-12 pct. In such operations, cadmium concentrations in blast furnace fume of from 3-5 pct are readily .attainable. However, the concentration gain beyond this range, with each additional circulation, is progressively decreased as a result of mounting losses occurring through handling and in end products. Therefore, to avoid excessive cadmium loss and to enhance the ultimate concentration anttainable, it is customary practice to isolate blast furnace fume at some intermediate cadmium content for special concentration procedure. The most common type cadmium concentration "campaign" involves special smelting operations wherein a relatively high portion of blast furnace fume at 3—6 pct cadmium is incorporated into the sinter charge. This type practice is roughly illustrated by the diagram on p. 111. Cadmium fume collected from lead blast furnace operations is not amen-

Jan 1, 1950

By K. E. Brown, G. H. Fancher

An 8,000-ft experimental field well was utilized to conduct flowing pressure gradient tests under conditions of continuous, multiphase flow through 2 3/8-in. OD tubing. The well was equipped with 10 gas-lift valves and 10 Maihak electronic pressure recorders, as well as instruments to accurately measure the surface pressure, temperature, volume of injected gas and fluid production. These tests were conducted for flow rates ranging from 75 to 936 B/D at various gas-liquid ratios from 105 to 9,433 scf/bbl. An expanding-orifice gas-lift valve allowed each flow rate to be produced with a range of controlled gas-liquid ratios. From these data an accurate pressure traverse has been constructed for various flow rates and for various gas-liquid ratios. A comparison of these tests to Poettmann and Carpenter's correlation indicates that deviations occur for certain ranges of flow rates and gas-liquid ratios. Numerous curves are presented illustrating the comparison of this correlation with the field data. Poettmann and Carpenter's correlation deviates some for low flow rates and, in particular, for gas-liquid ratios in excess of 3,000 scf/bbl. These deviations me believed to be mainly due to the friction-factor correlation. However, Poettmann and Carpenter's correlation gives excellent agreement in those ranges of higher density. This was as expected and predicted by Poettmann. He pointed out that their method was not intended to be extended to those ranges of low densities whereby an extreme reversal in curvature occurs.l As a result of these experimental tests, correlations using Poettmann and Carpenter's method were established between the friction factors and mass flow rates which are applicable for all gas-liquid ratios and flow rates. Definite changing flow patterns do not allow any one correlation to be accurate for all ranges of flow. INTRODUCTION The ability to analytically predict the pressure at any point in a flow string is essential in determining optimum production string dimensions and in the design of gas-lift installations. This information is also invaluable in predicting bottom-hole pressures in flowing wells. Although this problem is not new to industry, it has by no means been solved completely for all types of flow conditions. Versluys,2 Uren, et al, 3 Gosline,4 May,5 and Moore, et al,6,7 were all early investigators of multiphase flow through vertical conduits. However, all of these investigations and proposed methods were very limited as to their range of application. Likewise, many are extremely complicated and therefore not very useful in the field. Only in the last decade have any significant methods been proposed which are generally applicable. The most widely accepted procedure in industry at the present time is a semi-empirical method developed from an energy balance, proposed by Poettmann and Carpenter8 in 1952. Their correlation is based on actual pressure measurements from field wells. Accurate predictions from this correlation are limited to high flow rates and low gas-liquid ratios. Although this method will be discussed in detail later, it should be pointed out that two important parameters, namely the gas-liquid ratio and the viscosity, were omitted in their correlation. The viscosity was justifiably omitted since their data was in the highly turbulent flow region for both phases, and most wells fall in this category. The gas-liquid ratio was incorporated to some extent in the gas-density term. In 1954, Gilbert9 presented numerous pressure gradient curves obtained from field data for various flow rates and gas-liquid ratios for the determination of optimum flow strings. However, no method is presented for predicting pressure gradients except by comparison to these curves. Baxendell, et al,10 proposed a method based on Poettmann and Carpenter's procedure

By R. C. Earlougher, F. G. Miller, T. D. Mueller, H. J. Ramey

There are many studies of flow in radial systems that can be used to interpret unsteady rerervoir flow problems. Although solutions for systems of infinite extent can be used to generate solutions fur finite ow systems by superposition, application is tedious. In this paper a step is made toward simplifying calcu1ations of such solutions for finite flow systems. Superposition is used to produce a tabulu-lion of the dimension1e.s.s pressure drop function at several locations within a bounded square that has a well at its center. The square system provides a useful building block that may be used to generate flow behavior for any rectangular shape whose sides are in integral ratios. Values of the tabulated dimensionless pressure drop function are simply added to obtain the dimensionless pressure drop function for the desired rectangulm system. The rectangular system may contain any number of wells producing at any rates. Furthermore, the outer boundaries of the rectangular system may be closed (no-flow) or they may he at constant pressure. Mixed conditions also may be conyidered. Tables of the dimensionless pressure drop function for the square system are presented and various applications of the technique are illustrated. Introduction In 1945, van Everdingen and Hurst' published solutions for the problem of water influx into a cylindrical reservoir. Since this problem is mathematically identical with the depletion of a cylindrical reservoir with a well at the origin, the van Everdingen-Hurst solution may be used to study the depletion problem. In their analysis, they assumed that the fluid had a small, constant compressibility such that flow was governed by the diffusivity equation For a constant production rate q starting at time zero, van Everdingen and Hurst showed that the unsteady pressurc distribution for both finite and infinite systems could be expressed in terms of a dimensionless pressure 'Sabulations of the dimensionless pressure drop for a unit value of r, were provided by van Everdingen and Hurst,' and later by Chatas.' Others also presented values in graphical or tabular form." If the radius of the well becomes vanishingly small, r,+ O, the line source solution may be used for Eq. 2 when infinite systems are considered. Eqs. 5 and 6 are excellent approximations for Eq. 2 under certain conditions: In 1954, Matthews, Brons and HazebroekV emonstrated that solutions such as Eq. 5 can be superposed to generate the behavior of bounded geometric shapes; i.e., the behavior of a bounded single-well system can be calculated by adding together the pressure disturbances caused by the appropriate array of an infinite number of wells producing from an infinite system. These wells are referred to as image wells. Matthews, Brons and Hazebroek considered systems containing a single well producing at a constant rate. This superposition can be represented analytically as

Jan 1, 1969

By Leslie F. Tedsen, Alan E. Flanigan, John E. Dorn

IT is necessary occasionally to use aluminum-alloy sheet where moderately elevated temperatures are encountered. Considerable attention has been directed toward determining the influence of "artificial aging" on the room-temperature properties of the precipitation-hardenable alloys, as testified by numerous company reports and by references 1 to 4. Investigations on the properties at elevated temperatures are few, however,5-7 and have not always covered the range of times and temperatures of greatest interest. The present investigation was instituted to overcome this deficiency. The work was done for the Office of Production Research and Development of the War Production Board, under the supervision of the War Metallurgy Committee, as a part of the "restricted" Project NRC-548. It has been released for publication by the Office of Production Research and Development. As is well known, the high-strength aluminum alloys achieve their remarkable properties as a result of precipitation-hardening. In production they are subjected to a solution heat-treatment followed by quenching, to retain the supersaturated solid solution. The solution treatment is followed by "aging" (precipitation-hardening) either at room temperature or at a suitable elevated temperature. A considerable increase in tensile and compressive yield stresses results from precipitation at room temperature ("natural aging"). Through the elevated-temperature process ("artificial aging") it is possible to obtain values of yield stress considerably higher than those attainable by natural aging. The increase in yield stress is accompanied by a smaller gain in ultimate tensile stress and by a decrease in elongation. During [TABLE I.-Sources of Materials Used in the Testing Program MATERIAL ORIGIN AND TREATMENT 24S-T Alclad.... From Lockheed stock. 24S-RT Alclad... Direct from mill. 24S-T80 Alclad.. 24S-O Alclad from Lockheed stock, solution-heat-treated (925°F., water quench) and aged at 375°F. for t0 t % hour. 24S-T8I Alclad.. 24S-T Alclad from Lockheed stock, plant stretched up t0 I per cent and aged t0 ± % hr. at 375°F. 24S-T86 Alclad.. 24S-RT Alclad from Lockheed stock aged 534 ± 34 hr. at 375°F. 6IS-W (bare).... From Lockheed stock. 6IS-T (bare) 6IS-W (bare) from Lockheed stock aged 8 hr. at 350°F. XB7SS-T Alclad. From Lockheed stock.] the first stages of artificial aging the yield stress increases steadily until it reaches a maximum value. In this condition the material is said to be "fully aged." Further exposure results in "overaging," attended by a steady decrease in yield stress. In the production of the artificially aged materials, temperatures and times are selected to achieve full aging. The following important characteristics are associated with the process: I. The higher the temperature, the more rapidly is the fully aged condition attained.

Jan 1, 1945

By C. Gatlin, C. E. Nemir

A common cure of lost circulation is the introduction of granular bridging agents into the mud system. Many materials, such as ground nut shells, are used for this purpose. If the trouble causing void (fracture, fissure, vug, etc.) is not too large, the granular agent forms a "bridge" across or within the opening. Successively smaller particles in the mud stream then accumulate on and/or within this bridge until normal filtration is finally established. The efficiency of many bridging agents has been studied in the laboratory using various slot testers.',' Many investigators have remarked that a granular bridging material should have the proper particle size distribution. With the exception of the broad range specified in the patent of Goins and Nash,3 here is apparently no definition as to what this distribution should be. A bridge may be initiated when several particles of lost circulation material lodge against each other in a fracture or other void. Smaller particles then may bridge the openings between the larger, previously bridged particles. This process continues until the voids become quite small and the problem becomes one of filtration. It would seem logical that an optimum particle size distribution exists, i.e., one containing the proper quantity of properly sized material to fill the successively smaller voids of the bridge. The filtration characteristics of drilling fluids may be subject to a similar analysis. It has been clearly demonstrated by many workers that the filtration behavior of various muds can be altered by particle size control.'.' Slusser, et al, divided filtration into three periods and showed that particle sizes affecting a given period did not necessarily affect other portions of the filtration curve. An analagous problem is the proper sizing of gravel, liner slots and screen sizes in various sand-exclusion problems. Here the situation is reversed in that a proper "void" size, rather than the size of the bridging agent, is sought. The classic work of Coberly 9 forms the quantitative basis for most sand-exclusion processes. It is interesting to note that, in general, Coberly's work has been overlooked by most drilling-mud researchers. Other investigators have made various studies of the effect of particle size distribution .on drilling-mud properties. As a part of their studies, Fancher and Oliphant reported 30-minute filtration loss of a variety of mixtures of particle sizes.'' Gates and Bowie noted an effect of particle size distribution on filtration, as well as on other physical properties.' MAXIMUM DENSITY THEORY A maximum density mixture has been mentioned as the possible solution for both lost circulation and mud filtration problems. Furnas 12 derived mathematically a method for obtaining maximum density of beds of packed solids, having either a given number of component sizes or a continuous gradation of sizes. This work was verified experimentally by Anderegg.13 or mixtures having a continuous grading of sizes, the interval between sizes is taken as successive screen sizes of interval 2 The ratio of the quantity of each size and the next smaller size is given by the equation Fig. I, number of size intervals of ratio 2 taken from Furnas' paper, gives the value of n + 1 for any given values of + and K, where K is the ratio of the diameter of the smallest particles to the diameter of the largest particles. Measurement by weight assumes, of course, constant density for all particle sizes. Choosing the quantity of the smallest particle size as a unit weight, the required weights of the successively larger interials are then r1 r2 r3 . ®1,2,3. Thus, the grading curve of a maximum density mixture represents a geometric pro gression of ratio r.

By Frank G. Norris, William C. Marshall

The term "total operation" is meant to include problems that cannot be answered from the standpoint of either the blast furnace or the open hearth separately but must be studied by considering the interrelations of these two processes. There are other ways of expressing this idea, such as reference to the blast furnace and the open hearth as an integrated process or by emphasizing the interrelation and interaction of the two processes. Much progress has been made in metallurgy and other fields by breaking complicated processes and reactions into simpler parts and studying each of these intensively. This intensive study frequently is done under the controlled conditions of the laboratory experiment. The entire process is understood better by this specialized study of each of its parts. This procedure is so satisfactory that an understanding of unit operations is a fundamental requirement of chemical engineering. Much discussion of the open-hearth process is in terms of one heat or one furnace. By this is meant that the conclusions apply to one furnace, wherever it may be. Furnaces seldom occur singly; they are located in groups and these groups are located in steel plants having characteristic blast-furnace equipment. Problems that are affected by the number of furnaces operating, by the number of blast furnaces in the plant and by the fact that the open- hearth shop is dependent on the bla furnace capacity rather than on its o needs for the amount of iron available among those which, in contrast to "u operations," we have chosen to call "to operations." Many of these problems, such as cha ing delays and the general mechani problem of material handling, are familiar that merely to define " total op ations" brings them to mind. These pr lems are of such importance that alrea they have received careful thought 2 study and probably will merit furt study. As will be shown later, these mechan problems are so intimately related metallurgical problems of total operati that the effect of certain changes cannot ascribed with certainty to either a mech ical or a metallurgical cause entirely. Although the problems coming under general term of "railroading" are inclu in the problems of total operations, ' others are selected for the discussion of paper, One of these is strictly a problem composition; the other is strictly a prob of tonnage production. The problem of phosphorus is pres whenever basic open-hearth slag is used the blast-furnace burden. This practice not secured universal acceptance chi because of difference in preference for h manganese or low-manganese pig iron hjgh-manganese (2.00 per cent) iron is to made, open-hearth slag as a source manganese is usually cheaper than m

Jan 1, 1943

By William C. Marshall, Frank G. Norris

The term "total operation" is meant to include problems that cannot be answered from the standpoint of either the blast furnace or the open hearth separately but must be studied by considering the interrelations of these two processes. There are other ways of expressing this idea, such as reference to the blast furnace and the open hearth as an integrated process or by emphasizing the interrelation and interaction of the two processes. Much progress has been made in metallurgy and other fields by breaking complicated processes and reactions into simpler parts and studying each of these intensively. This intensive study frequently is done under the controlled conditions of the laboratory experiment. The entire process is understood better by this specialized study of each of its parts. This procedure is so satisfactory that an understanding of unit operations is a fundamental requirement of chemical engineering. Much discussion of the open-hearth process is in terms of one heat or one furnace. By this is meant that the conclusions apply to one furnace, wherever it may be. Furnaces seldom occur singly; they are located in groups and these groups are located in steel plants having characteristic blast-furnace equipment. Problems that are affected by the number of furnaces operating, by the number of blast furnaces in the plant and by the fact that the open- hearth shop is dependent on the bla furnace capacity rather than on its o needs for the amount of iron available among those which, in contrast to "u operations," we have chosen to call "to operations." Many of these problems, such as cha ing delays and the general mechani problem of material handling, are familiar that merely to define " total op ations" brings them to mind. These pr lems are of such importance that alrea they have received careful thought 2 study and probably will merit furt study. As will be shown later, these mechan problems are so intimately related metallurgical problems of total operati that the effect of certain changes cannot ascribed with certainty to either a mech ical or a metallurgical cause entirely. Although the problems coming under general term of "railroading" are inclu in the problems of total operations, ' others are selected for the discussion of paper, One of these is strictly a problem composition; the other is strictly a prob of tonnage production. The problem of phosphorus is pres whenever basic open-hearth slag is used the blast-furnace burden. This practice not secured universal acceptance chi because of difference in preference for h manganese or low-manganese pig iron hjgh-manganese (2.00 per cent) iron is to made, open-hearth slag as a source manganese is usually cheaper than m

Jan 1, 1943

By L. C. Brown, A. J. Stewart

Phase transformations have been studied in Ag-Zn alloys quenched from the high-temperature bcc 0 phase and lying in the composition range 37.4 to 50.0 at. pct Zn. On quenching, the alloy with the lowest zinc content transformed to massive a (fcc); all other alloys formed the ordered (3' phase. On deformation, a martensitic reaction took place forming a close-packed structure. At Lou' zinc contents transformation to this structure was complete. However, above 43 at. pct Zn a p.rogressively increasing amount of ß' was retained following deformation. The close-packed structure was fcc at lower zinc contents (under 47 at. pct Zn) and either hcp or a mixture of fcc and hcp at high zinc concentrations. The structures produced by cold working were unstable and on aging transformed to the ß' phase or the complex hexagonal to phase. For low zinc contents (under 43 at. pct) the fcc st-ructure transformed directly to the equilibrium To phase. With higher zinc contents, some 13' was retained following defownation, and on aging the amount of this phase relative to the close-packed structure increased. On further aging both structures transformed cornpletely to PO. Metallographic examination indicated that the nature of the deformation product depended very markedly on the mode of deformation. Tensile deformation gave a microstructure characteristic of thermal martensite. KING and Massalski1 have shown that an alloy of Ag-50 at. pct Zn quenched from the high-temperature bcc ß phase undergoes a low-temperature ordering reaction forming ß' which can be retained to room temperature. On deformation an hcp phase is produced, although this is unstable and the structure reverts completely to ß' on aging. In the present paper, the work of King and Massalski is extended to cover a wide composition range in the p phase, observations being made of the structure of the quenched 13 and of the effects of deformation and aging. The relevant portion of the Ag-Zn phase diagram is shown in Fig. 1. King and Massalski have shown that close to stoichiometry the ß' phase is the equilibrium structure at low temperatures. The approximate composition range of this phase, taken from a recent paper by Pops and Massalski,3 is shown on the phase diagram. The locations of atom sites are very similar in the ß' and to structures, and the 4, structure can be derived from the 0' structure by a small movement of atoms mainly in the direction of the cube diagonal.4'5 However, the probability of filling any particular atom site by a silver or a zinc atom is markedly different in the two structures. The structure can be considered partly ordered but the arrangement of the ordered atoms is completely different from that in the p' structure and transformation from ß' to requires a large fraction of the atoms to change position. It has been shown that the ß' transformation is thermally activated involving normal nucleation and growth processes.5,8 Massalski and Barrett7 have shown that in the Cu-Zn binary the (3 phase can be retained in the ordered state to room temperature over a wide composition range. On deformation a new close-packed phase is produced, the structure varying from fcc to a mixture of fcc + hcp to hcp alone with increasing zinc concentration. It appears that an ordering reaction is necessary to retain the bcc phase to room temperature. In CU-Ga,8 the bcc phase cannot be retained to low temperatures as it transforms by a massive reaction above the ordering temperature of the ß phase. The structure of the massive phase is very similar to that in Cu-Zn, varying from fcc to fcc + hcp to hcp with increasing zinc concentration. Similar structures have also been observed in CU-A1,9 Ag-Cd,10,11 and Ag-Al.12 EXPERIMENTAL The alloys were prepared by melting fine silver (99.99 pct purity) and electrolytic zinc (99.999 pct

Jan 1, 1969

By J. S. Kennedy, A. A. Lerew, C. M. Judson, G. L. Simard

DITHIOPHOSPHATE collectors are commonly used in the flotation of sulphide minerals. Studies of the interaction of a typical dithiophosphate collector with galena surfaces have been previously reported from. these laboratories." These fundamental studies were carried out by employing phosphorus labeled radioactive dithiophosphate. Radioactivity determinations then could be used to measure readily and accurately the small concentrations of dithiophosphate that, are present under conditions of flotation processes. Measurements were made on ground mineral, determining the amount sorbed indirectly from the concentrations in solution; and studies were also made with single crystals, determining the amount sorbed directly by counting the crystal surface. The rates, isotherms and reversibility characteristics of dithiophosphate sorption, the competition between phosphate and dithiophosphate for the mineral surface, and the exchange of sorbed dithiophosphate with dissolved dithiophosphate were studied. These studies have now been extended by sorption measurements in flotations with a Fagergren, machine. For this work, the selective flotation of galena and sphalerite from quartz was chosen, using ammonium di-(sec-butyl) dithiophosphate as. the collector, sodium cyanide as depressant for sphalerite, and copper sulphate as an activator for sphalerite. While the selective flotation of galena and sphalerite using a single dithiophosphate collector is not typical of flotation practice (two different collectors are generally used), it was found that a reasonably good separation could be obtained by using zinc sulphate with the sodium cyanide in the galena flotation and by cleaning the sphalerite concentrate or by carrying out the sphalerite. flotation in an alkaline medium. Data of practical importance on the distribution of collector between the concentrates, tailings, and solutions were obtained, particularly with regard to the effect of copper sulphate and sodium cyanide. In addition to the. selective flotation of galena and sphalerite from quartz, single flotations of galena-quartz and sphalerite-quartz mixtures were carried out, along with blank flotations on quartz alone. The present paper describes the results of these experiments. As in previous papers, the term sorption is used to designate uptake of collector by the mineral, without implication as to the nature of the processes involved. Experimental Materials: The mineral system was a ground synthetic mixture of galena, sphalerite, and quartz. The galena was from Galena, Kans., and contained 75 pct lead (theoretical 85.6 pct Pb for PbS); the sphalerite, from Ottowa County, Okla., contained 63 pct zinc (theoretical 67.2 pet Zn for ZnS) ; and the quartz from Klondike, Mo., analyzed as 99.97 pet SiO2. Sulphur labeled radioactive di-(sec-butyl) dithiophosphate was prepared from S82 supplied by the Oak Ridge National Laboratory on allocation from the U. S. Atomic Energy Commission. The synthesis consisted of precipitating barium sulphate, reducing the barium sulphate to barium sulphide, acidifying to form hydrogen sulphide, and oxidizing the hydrogen sulphide with iodine to elemental sulphur.

Jan 1, 1952

By Frank C. Appleyard

Gypsum, the dihydrate form of calcium sulfate, has a history of usefulness to man dating back several thousand years, and a worldwide industry has been built on the mining and processing of this versatile industrial mineral. However, anhydrite, the other principal calcium sulfate mineral has very limited use, so much so that separate statistics for it are not always kept, but are usually included with those for gypsum. Although often found in close association, the two minerals have important chemical differences in that anhydrite is the anhydrous form of calcium sulfate (CaSO,) whereas gypsum is the dihydrate (CAS0;2H20). These two molecules of combined water result in significant differences in hardness, density, and solubility of the two minerals. However, of most importance is the difference in thermal properties wherein gypsum, upon the application of a modest amount of heat, can be converted to the hemihydrate of calcium sulfate (CaS0;Vi H,O) or plaster of paris, an intermediate product upon which is based over 90% of the value of all calcium sulfate end products. Anhydrite, on the other hand, is inert at these temperatures and its uses have been limited to only those few cases where calcium sulfate in the anhydrous form may have an advantage. The earliest known use of gypsum plaster dates back some 5000 years to the time of the Pharaohs of Egypt who had discovered that gypsum rock, when exposed to fire, broke down into a powder which when mixed with water would form a putty that could be "plastered" on a rough mud brick or stone wall to make a smooth finish. It was used down through the centuries in a limited way for ornamental purposes, but did not achieve wide acceptance because of its quick (25 to 30 min) setting or hardening time which made it difficult to use. The first real understanding of gypsum chemistry was developed in France about 1755, and the gradual growth of its present utilization dates from that time. In the United States, the first utilization of gypsum was to grind it to a fine material for use as a soil conditioner at about the time of the Revolutionary War, and the term "land plaster" for ground gypsum has remained in use. Another cementituous material-lime or calcium oxide-had become the usual plastering material, but by about 1870 a method for retarding the set of gypsum plaster was discovered and it has today almost completely replaced lime as a plastering material. In recent years, gypsum products sold in the United States have reached a total valuation of approximately $500 million per year as illustrated in [Table 1].

Jan 1, 1975

By J. S. Kennedy, G. L. Simard, A. A. Lefrew, C. M. Judson, R. B. Booth

DITHIOPHOSPHATE collectors are commonly used in the flotation of sulphide minerals. Studies of the interaction of a typical dithiophosphate collector with galena surfaces have been previously reported from these laboratories.'* These fundamental studies were carried out by employing phosphorus labeled radioactive dithiophosphate. Radioactivity determinations then could be used to measure readily and accurately the small concentrations of dithiophosphate that are present under conditions of flotation processes. Measurements were made on ground mineral, determining the amount sorbed indirectly from the concentrations in solution; and studies were also made with single crystals, determining the amount sorbed directly by counting the crystal surface. The rates, isotherms and reversibility characteristics of dithiophosphate sorption, the competition between phosphate and dithiophosphate for the mineral surface, and the exchange of sorbed dithiophosphate with dissolved dithiophosphate were studied. These studies have now been extended by sorption measurements in flotations with a Fagergren machine. For this work, the selective flotation of galena and sphalerite from quartz was chosen, using ammonium di-(sec-butyl) dithiophosphate as the collector, sodium cyanide as depressant for sphalerite, and copper sulphate as an activator for sphalerite. While the selective flotation of galena and sphalerite using a single dithiophosphate collector is not typical of flotation practice (two different collectors are generally used), it was found that a reasonably good separation could be obtained by using zinc sulphate with the sodium cyanide in the galena flotation and by cleaning the sphalerite concentrate or by carrying out the sphalerite flotation in an alkaline medium. Data of practical importance on the distribution of collector between the concentrates, tailings, and solutions were obtained, particularly with regard to the effect of copper sulphate and sodium cyanide. In addition to the selective flotation of galena and sphalerite from quartz, single flotations of galena-quartz and sphalerite-quartz mixtures were carried out, along with blank flotations on quartz alone. The present paper describes the results of these experiments. As in previous papers, the term sorption is used to designate uptake of collector by the mineral, without implication as to the nature of the processes involved. Experimental Materials: The mineral system was a ground synthetic mixture of galena, sphalerite, and quartz. The galena was from Galena, Kans., and contained 75 pct lead (theoretical 85.6 pct Pb for PbS); the sphalerite, from Ottowa County, Okla., contained 63 pct zinc (theoretical 67.2 pct Zn for ZnS); and the quartz from Klondike, Mo., analyzed as 99.97 pct SiO,. Sulphur labeled radioactive di-(sec-butyl) dithiophosphate was prepared from SS supplied by the Oak Ridge National Laboratory on allocation from the U. S. Atomic Energy Commission. The synthesis consisted of precipitating barium sulphate, reducing the barium sulphate to barium sulphide, acidifying to form hydrogen sulphide, and oxidizing the hydrogen sulphide with iodine to elemental sulphur.

Jan 1, 1953

By J. S. Kennedy, A. A. Lefrew, C. M. Judson, R. B. Booth, G. L. Simard

DITHIOPHOSPHATE collectors are commonly used in the flotation of sulphide minerals. Studies of the interaction of a typical dithiophosphate collector with galena surfaces have been previously reported from these laboratories.'* These fundamental studies were carried out by employing phosphorus labeled radioactive dithiophosphate. Radioactivity determinations then could be used to measure readily and accurately the small concentrations of dithiophosphate that are present under conditions of flotation processes. Measurements were made on ground mineral, determining the amount sorbed indirectly from the concentrations in solution; and studies were also made with single crystals, determining the amount sorbed directly by counting the crystal surface. The rates, isotherms and reversibility characteristics of dithiophosphate sorption, the competition between phosphate and dithiophosphate for the mineral surface, and the exchange of sorbed dithiophosphate with dissolved dithiophosphate were studied. These studies have now been extended by sorption measurements in flotations with a Fagergren machine. For this work, the selective flotation of galena and sphalerite from quartz was chosen, using ammonium di-(sec-butyl) dithiophosphate as the collector, sodium cyanide as depressant for sphalerite, and copper sulphate as an activator for sphalerite. While the selective flotation of galena and sphalerite using a single dithiophosphate collector is not typical of flotation practice (two different collectors are generally used), it was found that a reasonably good separation could be obtained by using zinc sulphate with the sodium cyanide in the galena flotation and by cleaning the sphalerite concentrate or by carrying out the sphalerite flotation in an alkaline medium. Data of practical importance on the distribution of collector between the concentrates, tailings, and solutions were obtained, particularly with regard to the effect of copper sulphate and sodium cyanide. In addition to the selective flotation of galena and sphalerite from quartz, single flotations of galena-quartz and sphalerite-quartz mixtures were carried out, along with blank flotations on quartz alone. The present paper describes the results of these experiments. As in previous papers, the term sorption is used to designate uptake of collector by the mineral, without implication as to the nature of the processes involved. Experimental Materials: The mineral system was a ground synthetic mixture of galena, sphalerite, and quartz. The galena was from Galena, Kans., and contained 75 pct lead (theoretical 85.6 pct Pb for PbS); the sphalerite, from Ottowa County, Okla., contained 63 pct zinc (theoretical 67.2 pct Zn for ZnS); and the quartz from Klondike, Mo., analyzed as 99.97 pct SiO,. Sulphur labeled radioactive di-(sec-butyl) dithiophosphate was prepared from SS supplied by the Oak Ridge National Laboratory on allocation from the U. S. Atomic Energy Commission. The synthesis consisted of precipitating barium sulphate, reducing the barium sulphate to barium sulphide, acidifying to form hydrogen sulphide, and oxidizing the hydrogen sulphide with iodine to elemental sulphur.

Jan 1, 1953

By Grover J. Holt

IN order to provide a clear picture of the development of the sink-and-float process of concentration as applied to the iron ores of Minnesota, a few pertinent facts should be brought out concerning the ores and the products of concentration. Iron ore is primarily a cheap commodity handled in immense quantities. The price of iron ore at present, based on a natural iron content of 51.5 per cent, varies from $2.55 to $2.70 per gross ton f.o.b. cars at the mine or washing plant in Minnesota. Last year 92,000,000 gross tons were shipped from the Lake Superior district (Minnesota, Michigan, and Wisconsin) to the furnaces. Concentrated iron ores have no greater value per unit of iron content than ores that can be mined and shipped direct from the shafts or open pits. For years only the higher grades of concentrating ores could be treated and sold in competition with the immense reserves of direct shipping ore available. These higher-grade "straight wash" ores required only the simplest treatment; namely, the washing out of fine sand from coarse ore particles. As the exhaustion of the "straight wash" ore is reached, rock is found replacing part of this sand, and the ore no longer responds to the former sizing treatment. Substantial tonnages of this marginal (jig ore) remained to be treated. Because of the limitations placed on concentrates by the furnaces-namely, low price of product and minimum amount of fines-iron-ore concentration has been and must continue to be a one-pass process. Only an increase in price or a change in structure of concentrates allowed by the ore consumer will encourage departure from this practice. Faced with the necessity of handling large tonnages, with the limitations mentioned, iron-ore research men have found their search for new and more efficient methods of treatment seriously handicapped and removed from the field of fine crushing. Sink-and-float treatment appeared to offer the best field in coarse concentration and has been proved by several plants to be well adapted to our problem. The use of ferrosilicon as a medium solid was decided upon. In our present practice, the ferrosilicon metal, carrying about 83 per cent iron, 15 per cent silicon and 2 per cent carbon and nonmagnetics, is crushed to pass 65 mesh and used without further sizing. When mixed with water the specific gravity of the medium may be controlled to within 0.02 per cent above or below the required gravity. Table I shows examples of a change in solid content of the medium for varying gravities. [ ] Table I is based on clean ferrosilicon, whereas some contamination is always present in the mill circuit, tending to

Jan 1, 1943

By Blake M. Loring, Robert A. Colton

MELTING procedures for most metals and alloys usually include some provision for the control of oxygen, since this element frequently has some undesirable effect on the properties of the metal or alloy concerned. In the melting of the various bronzes, this is especially true, since oxygen can be introduced into the melt in a number of ways, most of which are difficult to control. In making bronzes from virgin materials, oxygen is usually present in the commercial grades of copper used; electrolytic he refined copper ingots usually contain from 0.02 to 0.05 per cent oxygen. When ingot metal or scrap bronze is used in the charge, oxides are almost always present to some degree. Under certain melting conditions and in certain types of melting equipment the atmosphere over the metal may be highly oxidizing. This, of course, may be desirable in the melting practice used, but is certain to introduce appreciable amounts of oxygen into the melt, and that may not be entirely desirable. From the foundry viewpoint oxygen may have several harmful effects on bronzes. The formation of excessive amounts of oxides may produce drossy metal, which, in turn, means dirty castings and a potentially high rejection rate. It is claimed, too, that oxides in the metal may combine with hydrogen to form steam and thereby produce porosity in certain of the bronzes. The presence of certain refractory oxides, such as SnO2, may be undesirable from the viewpoint of making machining difficult, or as possible stress-raisers in the metal matrix. It is often said that excessive oxide present in the liquid metal makes the metal run sluggishly. Since it appears impractical to try to control the amount of oxygen introduced into the metal beyond taking the economical limit of precaution about charging dirty scrap, it would seem that control of the oxygen content of the liquid metal offers the most promising approach to this problem. This might be done by using slags, or covers, or by the use of some element or compound added to the melt to remove oxygen preferentially. Most aspects of this problem have been considered and considerable work has been done along these lines. A reconsideration of the problem is indicated, however, by the controversial nature of the evidence at hand, especially on the possibility of using a chemical deoxidizer to control the oxygen content of bronzes. CHOICE OF DEOXIDIZER The choice of the chemical agent selected as a deoxidizer would naturally depend first on the alloy in which it is to be used; in this particular case the alloy is Navy gun metal. In Table I are listed a group of elements that might be considered as

Jan 1, 1946

By W. T. Isbell, Carleton C. Long

Zinc recovery from lead blast-furnace slags has heretofore been an indirect process, involving, first, the fuming off and collecting of an impure zinc oxide, and second, the reduction of the zinc portion of this oxide to metal either by electrolytic or pyrolytic means. (In a variation of this process, blue powder is the intermediate product rather than zinc oxide fume.) In 1940, W. T. Isbell proposed that molten slag from the lead blast furnace or stock-pile slag melted down in a blast or cupola-type furnace be charged directly into an airtight container (i.e., furnace) provided with means to heat further the slag by passage of electric current and means to introduce the carbon (coke) necessary to reduce the ZnO constituent of the slag to zinc as a zinc vapor and CO. He also proposed that the zinc vapors so obtained be condensed in a Weaton-Najariant internal condenser directly connected to the proposed furnace. It was thought that the Weaton-Najarian condenser could liquefy zinc vapor from lean mixtures of vapor and noncondensable gases. Such condensers have been in commercial use! since 1936 at Josephtown smelter, where the source of zinc vapor is a column of coke and zinc-bearing sinter electrically heated (charge resistor). Condenser output when supplied with vapor-gas mixtures containing approximately 45 per cent zinc and 55 per cent noncondensable gases, varies from 18 to 30 tons of slab zinc per day per condenser, depending upon the heat-transfer area (length) of the condenser and the volume of vapor (furnace size) fed to it. Lead-smelting operations at the St. Joseph Lead Company's plant at Hercu-laneum, Mo., produce a slag containing 12 to 16 per cent zinc. For several years this slag has been stock-piled with the object of recovering the zinc values if and when a commercial method was invented. Evaluation of the possibilities of the proposed method was made by pilot-plant operation at Josephtown. The first plant, designed in 1940 and operated in early 1941, consisted of a single-phase, two-electrode furnace. The evolved vapors were burned. Electrical characteiistics of the molten slag, power requirements, coke requirements, and extent of zinc elimination indicated the feasibility of the proposed method. In the latter part of 1941 a second pilot furnace was constructed, to which "was attached a small (6 ft. long) Weaton-Najarian condenser in order to develop an over-all picture of zinc-in-slag to zinc-in-slabs. This furnace was operated in the early part of 1942 and yielded such promising results that a decision was made to design- and construct a commercial furnace. Feed for the pilot-plant furnaces was granulated slag. A suitable deduction (300 to 350 kw-hr. per ton slag) was calculated in estimating power require-

Jan 1, 1944

By M. R. Hatfield, F. J. Vosburgh

IN a recent article,† it was shown that in the blast furnaces in Germany that are lined with carbon blocks no cooling plates are used, and that shower cooling is employed on the hearth and bosh sections. While one of the authors was in Germany he was told that one furnace was being operated without even the shower cooling on the bosh section, though the hearth section was shower-cooled. In discussion of this interesting situation with a number of blast-furnace operators in this country, it was made clearly and promptly evident that shower cooling was very unpopular, probably because of its messiness and its ineffectiveness. Both of the causes for the dislike of shower coolings are reasonable ones. Shower cooling can be and frequently is messy, but the present cooling of blast furnaces leaves much to be desired on that score. Shower cooling is ineffective as compared with plate cooling, so far as its usefulness in keeping the bricks cool enough not to melt or fall to pieces is concerned. However, the introduction of carbon linings changes the situation. No one is concerned with keeping a carbon lining cool, for no temperature in the blast furnace has any effect on carbon, which is just as stable at 3000°F. as it is at 70°F. The only concern is for the shell-to keep it cool enough for safety and comfort and for that shower cooling is sufficient. Of course, with only the shell to cool, instead of the shell plus all the refractory material, much less water would be required, and the necessity for constant attention to the flow would be lessened, as the hundreds of inlets and outlets would be eliminated. Probably half of the water used in cooling a blast furnace is used for cooling the shaft and tuyeres and the remainder for the bosh and hearth sections. However, in view of the dislike of shower cooling in the United States, and particularly because at least one German blast furnace is operated with no cooling of the bosh section, thought was given to the possibility that a carbon-lined blast furnace might be operated without any cooling of the entire carbon-lined portion. For that reason a series of experiments was performed to determine what might be the temperature of the shell of a blast furnace protected by a carbon lining and operated under varying conditions up to a maximum inside temperature of 3000°F. EXPERIMENTAL PROCEDURE A schematic diagram of the experimental setup is shown in Fig. I and a photograph of the entire assembly in Fig. 2. The heating element was a carbon tube nominally 2 5/8 in. o.d. by 2 in. i.d. by 30 in., used as a resistor. Power was furnished by a 15-kva. transformer operating

Jan 1, 1941

By M. E. Wadsworth, C. H. Pitt

Nickel corrosion in sulfuric acid solutions at elevated temperatures and oxygen wer-pressures was imestigated. Weight loss was 1inear with time and varied directly with oxygen concentration. Independent variation of the possible active species in solution indicated that the undissociated sulfuric acid molecule plays an important part in the corrosion mechanism. The rate determining step was considered to be the adsorption of oxygen on a site containing adsorbed H2SO4. THE tendency for a metal to go into solution depends on a number of factors some of which are: 1) the position of the metal in the electrochemical series; 2) the type and concentration of corroding species in solution; 3) the concentration of oxygen in solution; 4) the type of film formed at the liquid-metal interface; and 5) the physical state of the metal. The corrosion of a metal in an aqueous solution may be considered to be a heterogeneous reaction that occurs at the liquid-metal interface. The reaction is generally considered to occur as a result of electrochemical potential differences within the system. Little work has been published in the literature concerning the corrosion of pure nickel. A great deal has been publistled dealing with the experimental and theoretical aspects of the over-all corrosion process. Evans,1 Uhlig,' and recently Todt 3 and Tomashoff,4 have published books which review the results of experiments which have been conducted on corrosion, and have developed some of the basic ideas of the more widely accepted theories of corrosion. Friend5 states that. nickel does not readily discharge hydrogen from any of the common nonoxidiz-ing acids and that a supply of some oxidizing agent is necessary for appreciable rates of corrosion. He further notes that at temperatures between atmospheric and close to boiling, corrosion rates tend to vary with concentration, temperature, and aeration in acid concentrations up to 25 pct. Whitman and Russel6 studied the effect of dissolved oxygen on a number of metals in acid solutions and found that oxygen accelerates the rate of corrosion of nickel in sulfuric acid. Flowers and Kelley7 in studying the action of dissolved CO, on electroplated nickel postulated that nickel dissolves as NiHCO3 in the presence of CO, and air. It was found that oxygen was necessary for corrosion to take place and that the rate increased with increasing amounts of oxygen in solution. Flowers and Kelley attributed the oxygen effect to cathodic depolarization. MacGillavry, Rosenbaum, and wensson' determined metal solution potentials of nickel in various electrolytes. They found that nickel has no tendency to corrode in alkaline solutions in the presence or absence of air. In acid solutions in the presence of air, metal solution potential increases in the order of 1/2 v were observed. This increase was attributed to probable chemisorption of oxygen on the nickel surface and the corrosion mechanism suggested was the interaction of H+ ions with the nickel oxide formed at the surface. Delahay9 observed the reduction of oxygen on various metals. A polarograph was used to measure the course of the reaction. With some metals hydrogen peroxide was produced as an intermediate compound. However, nickel was not considered to be a hdrogen peroxide producer. Van Rysselberghe 10,11 and associates attributed the accelerating effect of carbon dioxide on the corrosion process to the presence of percarbonic acid produced in solution reacting with the hydrogen peroxide. The percarbonic acid can be reduced at less negative potentials than hydrogen peroxide and as a result accelerates the reaction. EXPERIMENTAL Since a complete description of the apparatus used can be obtained elsewhere,12'13 no attempt will be made here to describe the equipment other than to note that it consisted essentially of an autoclave unit from which samples could be withdrawn periodically without disturbing the interior state of the autoclave. A titanium autoclave liner was used to protect the autoclave from the solution.

Jan 1, 1961

Alfred Stansfield, Montreal, Canada:—In Professor Howe's paper on the position of Ae3, he shows its industrial importance in determining the temperature to which steel should be heated for " grain refining." Several years ago I carried out a research on the " burning " of steel and found that while hypo-eutectoid steel should be heated to Ae3, hyper-eutectoid steel that has been very much overheated must be reheated to the curve Sa on the carbon-iron diagram, in order to redissolve the pro-eutectoid cementite and thus to obtain recrystallization and grain-refining. This treatment was necessarily only partly successful, and I should like to ask whether the conditions of heat treatment for refining overheated high-carbon steels have been ascertained. Speaking of the &'Persistence of Solidificational Segregation " Professor Howe quotes an experiment made by Mr. Stead in which a bar of 1.2 per cent. carbon steel was immersed in a large mass of molten blast-furnace slag and allowed to cool with it. The steel was heated ; above the solidus (curve An on the carbon-iron diagram), but below the liquidus (curve AB). A drop of eutectic carbon-iron alloy, rich in carbon, had liquated out and hung below the bar. This agrees exactly with my own observations on the burning of steel, but my interpretation differs somewhat from that of Professor Howe. Professor Howe considers that the fusion of a part of the metal (rich in carbon) shows that the solidificational irregularities of composition had persisted through the rolling and heat treatment of the steel, as otherwise no part of the steel would have been sufficiently fusible to melt. It does not appear to me that such an explanation is necessary. A piece of steel represented in temperature and composition by any point within the area ABa will ultimately resolve itself into a solid phase and a liquid phase in equilibrium with each other. It may appear that if the steel were absolutely uniform no fusion could take place, but, the smallest nucleus of high-carbon, fusible alloy would ultimately bring about this separation into liquid and solid phases, by diffusion of the carbon from the solid to the liquid areas. A nucleus sufficient for the purpose might be provided by an area of pro-eutectoid cementite which had not become diffused during the

Jan 1, 1914

By Oscar Weiss

STILFONTEIN and surrounding areas gave nega-tive results in all prospecting attempts since about 1904 when Goerz and Co., a forerunner of Union Corporation Ltd., first drilled in the region and on the farm Stilfontein. Subsequent efforts by African and European Investments Co. and Anglo American Corp. from 1934-37 were completely unsuccessful. Holes drilled by these companies on the farms Riet-fontein, Hessie, and Palmietfontein were stopped in the Lower Witwatersrand system without finding payable reefs. The results of gravimeter, ground magnetometer, and aerial magnetometer surveys are presented in the area, in and around the new Stilfontein Gold Mine, in the Klerksdorp District of the Transvaal in the Union of South Africa. The gravimeter and ground magnetic surveys were completed in 1947—48. The gravity anomalies suggested a block of Upper Witwatersrand quartzites faulted-up between denser rocks of dolomite and Ventersdorp lava. Boreholes S.T. 1, 2, and 3 were drilled in 1948 and, after penetrating the dolomite and Ventersdorp lava, entered Upper Witwatersrand quartzites and intersected the Gold Estates Reef and Vaal Reef. Subsequent drilling delineated the suboutcrop of the Vaal Reef and determined the main structure of this horizon. The gold content of the Vaal Reef was highly payable and shaft sinking is now in progress. The Stilfontein Gold Mining Co. has been formed and, up to date, f5,000,000 capital has been raised for plant, shaft sinking, and development. The payable Vaal Reef horizon extends further south from Stilfontein, the reef occurring at increasing depths. It is possible that at least another mine may be established on these deeper horizons. The farm Stilfontein 39 is situated in the Klerksdorp District of the Transvaal. This farm and the surrounding areas have been subjected to repeated programs of prospecting dating back to about 1904, when Goerz and Co., the forerunner of Union Corporation, Ltd., first drilled on the farm and in the surrounding areas. From 1934-37, numerous boreholes were drilled on the neighboring farms, Riet-fontein. Hessie. and Palmietfontein, by African and European Investment Co. and Anglo American Corp. All these efforts were completely unsuccessful, and nobody suspected any possible gold-bearing area on Stilfontein until about 1947, when a gravity traverse run by B. D. Maree on the main road, showed a negative gravity anomaly. During 1947-48, the writer's organization completed gravimeter and magnetic surveys on Stilfontein and Rieffontein. An area of negative gravity anomalies was mapped, and it was suggested that this could be caused by blocks of Upper Witwatersrand quartzites, of the average density of 2.65, faulted up between dolomites and Ventersdorp lavas, the density of both of these rocks being 2.8. Fig. 1 shows the geology of the area as mapped by L. T. Nel of the Geological Survey of South Africa. The boreholes on Stilfontein, with the exception of a single hole of Goerz and Co., were drilled after the completion of the geophysical survey. The grouping of the first boreholes S.T. 1, 2, 3, 4, 5, and 6, clearly shows that these were located in the zone of negative gravity anomalies. Fig. 2 shows the gravity anomaly contours. Fig. 3 shows two sections across the gravity anomaly, together with the corresponding geological sections as obtained from boreholes. The close relation between gravity values and thickness of dolomite plus Ventersdorp lavas is striking. The two latter formations having the same density (2.8), act as one mass as far as gravity effects are concerned. Fig. 4 shows the magnetic anomalies observed on the ground by vertical magnetometers and at 500 ft abbve mean ground level by aerial magnetometer. The latter are anomalies of the total magnetic intensity. The magnetic results show that, on the farm Rietfontein and on the northern half of Stilfontein. Lower Witwatersrand magnetic shales were to be expected at relatively shallow depths. As the strongly

Jan 1, 1952

By Robert Maddin

THE application of electrolytic polishing of metals introduced a new technique for preparing surfaces, especially for single crystals. This procedure has generally been assumed to eliminate the strain introduced by mechanical polishing and to result in a more truly representative surface, particularly in the case of soft metallic materials. However, apparently little information is available concerning specific characteristics of a surface prepared electrolytically. The conventional method of mechanical polishing is known to produce a layer of distorted metal which is usually removed by a suitable chemical etchant. To what depth the strain introduced by mechanical polishing penetrates into the lattice is still obscure. The present investigation illustrates the apparently anomalous appearances of glide ellipses on electrolytically polished surfaces of aluminum single crystals. EXPERIMENTAL PROCEDURE AND RESULTS Aluminum single crystals, 99.975 pct pure, remaining from the investigation of Found,1 were polished electrolytically using a solution of fluoboric acid and a low current density. Laue back-reflection technique, interpreted after the manner of Greninger,2 was used to determine the orientation and the specimen axis rotation of the crystals. Three flat surfaces about 4 mm wide parallel to the specimen axis, one perpendicular to the theoretical slip direction and the other two 1200 apart, were polished mechanically and repolished electrolytically. A tensile load was applied using a Southwark-Emery tensile machine at a rate of about 40 lb per min. Elongation was measured by noting the initial and final gauge lengths. X ray diffraction was used to obtain the usual X and X values in order to calculate the elongation and shear by plotting stereographically the specimen axis rotation by means of the Schmid-Boas formula.3 In Table I may be found the value of the gauge diameter, measured elongation, calculated elongation and shear for the crystals investigated. Fig 1 shows the initial and final positions of the specimen axes of the crystals. [ ] At a low magnification the slip lines developed on specimen Al-I appeared straight and rather evenly spaced. However, at a high magnification, the slip lines were seen to be composed of small markings which were present throughout the length of the specimen (Fig 2). The distance between the markings was fairly constant and their directions all parallel to one another. Fig 3-5, photographed on different surfaces of the specimen, illustrate the interesting appearance of these lines. It may be noticed from Fig 4 that the markings, which present the appearance of

Jan 1, 1948