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By S. Beatty

RECENT experimental results' on the superconductive properties of vanadium indicate that the magnetic behavior of the metal is greatly affected by internal strains caused by mechanical work, and particularly by oxygen and nitrogen impurities. These result in an increase in the hardness of the metal such that metallurgists' have used hardness as a measure of the impurities. An increase in the impurities should also be reflected in a change of lattice parameter with increasing impurity content. The lattice parameter of vanadium prepared by the thermal decomposition of the iodide has been determined by two workers. Neuburger3 obtained a value of a, =3.0338 ± 0.0003A for the body-centered cubic lattice by means of the powder method. The work of Katelaar is referred to by van Arkel4 in which a value of a0 = 3.025 is given. Four samples were used for this investigation. Sample A, the vanadium of the highest purity in the group, was obtained by means of the thermal decomposition of vanadium diiodide and deposited on a 3 mil diam tungsten filament in the form of crystals. The second sample, labeled B, was obtained by the calcium reduction of the pentaoxide at a sufficiently high temperature to give a melt. A third sample, C, was obtained in the same manner as B but remelted in a pure argon atmosphere. The last sample, D, was prepared by the calcium reduction method and the fine powdered vanadium was then sintered by means of applied heat and pressure. Samples A, B, and C were thus essentially free of mechanical strain in their preparation. Sample D was annealed in a high vacuum at 800°C. The samples were prepared for X-ray diffraction analysis such that all additional strain by cold work or by contamination with oxygen and nitrogen was kept at a minimum. Powder obtained from filings was deemed unsuitable since this would require annealing to get rid of the cold work. A heat treatment up to 1000°C at 10-6 m pressure might still increase the impurity content by means of adsorbed oxygen from residual gas in the vacuum chamber. The most satisfactory samples were prepared for back-reflection film techniques. Samples were cut to size, etched with hydrobromic acid, and mounted in Bakelite. They were then lightly polished on 3-0 paper and lightly etched. Chemical and Hardness Analysis of Samples Spectrographic analyses were made of the four samples and indicated similar metallic impurities for the group. The major metallic impurity in each sample was iron, which was less than 0.01 pct. The sum of the other metallic impurities was approximately 0.1 pct. The carbon content was assumed low by virtue of the methods of sample preparation. The principal impurity difference between the samples was in the oxygen and nitrogen content.

Jan 1, 1953

By D. Turnbull, R. E. Cech

THE supercooling behavior of pure liquid metal droplets has been described.' The solidification behavior of small droplets of Cu-Ni alloys as a function of composition is described herein. The Cu-Ni system is of interest for such an investigation because the components are miscible in all proportions in both the liquid and solid state and the phase diagram of the system, Fig. 1, is a type often encountered in metal systems. It was noted by Van Riemsdyk2 and others that the nature of the "blick" of gold droplets during assaying is not perceptibly affected by the content of the platinum group metals that are soluble in both liquid and solid gold. With the exception of these very qualitative observations there appear to have been no prior investigations of the supercooling of alloy droplets. A series of nine alloys varying in composition by 10 pct (nominal weight) steps was made using certified OFHC copper, 99.996 pct purity, obtained from the American Brass Co., and electrolytic nickel pellets, 99.92 pct purity, obtained from the International Nickel Co. The alloys were melted and cast in vacuo in a high frequency induction furnace. Segregation was minimized by chill casting into 1-in. diam steel molds. Each alloy rod was homogenized at a temperature 50°C lower than the solidus for 100 hr in dry hydrogen. Samples for solidification experiments and chemical analysis were machined from the same portion of each rod and at a depth of in. from the rod surface. A Car-boloy tool was used in taking turnings to minimize contamination of sample by the cutting tool. As a check, a number of samples for microscopic observation were chipped from the ingot with a fragment of pyrex glass. The resultant data in all cases agreed, within experimental error, with the data obtained from machined turnings. A number of small particles, 30 to 50 micron diam, of a Cu-Ni alloy were placed in a quartz vial 1/32 in. diam x % in. long. This was inserted into a platinum ribbon heater and mounted in a high temperature microscope stage. The general procedure followed in inserting samples into the stage and measuring the temperature of melting and solidification was the same as described in an earlier paper.' A chromel-alumel thermocouple was used to study alloys of 88.93 pct Cu, 80.62 pct Cu, and 72.27 pct Cu. A platinum-10 pct rhodium thermocouple was used for the remainder of the alloys. Procedure The assembled high temperature microscope stage was first evacuated and the sample given a 2 min in situ treatment at 900 °C in dry hydrogen to remove surface oxides which might otherwise catalyze crystal nucleation. After this treatment the atmosphere was changed to purified helium and melting and solidification were observed microscopically. It was not possible to determine the solidus with certainty. However, the liquidus temperature was measured very accurately since the surface of the particle changed in appearance from coarse and uneven to smooth, mirror-like within a few degrees. The visually determined liquidus temperature was checked by finding the highest temperature to which the particle could be heated such that it did not supercool upon lowering the temperature. This temperature which checked within experimental error with that found by observing surface change was assumed to be characteristic of the thermody-namic liquidus. In order to minimize the effect of selective evaporation of copper from the alloy, samples were changed frequently and the droplets were heated no more than 50 °C in excess of the liquidus temperature T,. When the latter conditions were fulfilled, T, values were reproducible. After melting, the temperature was decreased slowly until the particles solidified. The sudden release of heat of fusion on solidification caused the

Jan 1, 1952

By T. S. Lundy, R. A. Padgett

The fact that cobalt diffuses in silver at a much slower rate in a region near a free surface than in bulk material has been demonstrated in a variety of experiments. Various possible mechanisms of this near-surface effect (NSE) are examined in light of experimental evidences. The tendency for surface segregation of some solute atoms appears to be a likely mechanism to explain the effect. UNIDIRECTIONAL and isothermal diffusion from a plane source of radioactive tracer into an isotropic, homogeneous medium follows the Gaussian solution to Fick's second law, or: where A(x,t) is the position and time-dependent concentration of the diffusing species, M is the quantity of diffusant per unit area initially at x = 0, and D is the diffusion coefficient. For a given time, say t = tl, one can easily see that: d In Aixji)_____1_ r2] d(x2) 4Dti Thus, if diffusion data obtained by serial sectioning are plotted as In A(x,tl) vs x2, the diffusion coefficient is obtained from Eq. [2]. The ideal behavior seldom is observed in real systems. Deviations from ideality generally occur either at small or large values of penetration distance. The overall picture is shown schematically in Fig. 1 where Regions I, 11, and 111 are due, respectively, to some near-surface effect or effects (NSE), volume diffusion, and short-circuiting effects. For different systems and conditions of specimen preparation and analysis, the relative importance of Regions I, 11, and I11 may be drastically different. Region I is completely absent in many systems and there is no NSE. In others, however, there may be considerable difficulty in determination of volume diffusion coefficients due to the overshadowing influences of Region I. Such is particularly true when indirect techniques such as the surface concentration decrease or the Gruzin method' are used to find D. In this paper several experiments which had as their goal a better understanding of near-surface effects are reported. Specifically, it is well-known that unusual penetration behavior results for the diffusion of several impurities in ilver- and that considerable controversy exists with regard to interpretation of the published diffusion data. We chose to examine those unusual results which occur for cobalt diffusion in monocrystalline silver395 primarily because knowledge of experimental procedures and materials were readily available. Both radioactive co60 and co5' could be utilized to offer a wide range of available concentration of the diffusing species. Experiments were also performed on the diffusion of AgnO in silver. They gave base-line data for the system—both for technique evaluation and for examination of the vacancy distribution near the surface. I) PROCEDURES Cylindrical-shaped specimens 1.25 cm diam and 1 to 1.25 cm long were cut from 99.999 pct Ag single crystals obtained from Monocrystals Co., Cleveland. One end surface of each specimen was polished flat and etched with a mixture of 20 ml saturated Cr03 solu-tion-20 ml H20-3 ml concentrated HC1. Radioactive tracer (co60 or co5' or Ag'lO, each having a radio-chemical purity of greater than 99 pct) was deposited onto the prepared surface either dropwise with evaporation to dryness of the solution containing the tracer (0.5 N HC1 solution for the co60 and co5' and 0.6 N HNO3 solution for the A"'), by electroplating, or by evaporation from a tantalum or tungsten filament in an evacuated bell jar. The amount of deposited cobalt was varied from many atomic layers of cobalt containing the co60 to approximately one co5' atom per lo6 surface atoms of silver. This large variation in amount of deposited cobalt yielded information about both the influence of a thick-source layer of tracer and solubility effects on the NSE. Such variations were possible because of the large differences in half-lives,

Jan 1, 1969

By E. R. Gilbert

Klopp et al. have reported data on tensile and creep properties of are-melted and electron-beam-melted tungsten. We would like to point out some similarities between their creep results and ours on are-melted and powder-metallurgy tungstenand offer some alternate interpretations of the data which lead to different rate-controlling mechanisms. Klopp et al. observed extensive transient creep in the 2250" to 3500°F temperature range where the acthetivation energy is 106,400 ± 3300 cal mole-1. They suggest cross slip as the possible rate-controlling mechanism since "cross slip may occur only by the movement of screw dislocations, and not edge dislocations, thus allowing only partial recovery of the strain hardening and resulting in a continuously decreasing creep rate, characteristic of transient creep.'' Our tests on are-melted tungsten and powder-metallurgy tungsten displayed an extensive transient creep stage in the same temperature range but they also displayed a steady-state creep stage. The stress levels and strain rates of the two investigations, 1.4 to 7 kg mm-2 and 10-7 to 10-4 sec-1 for that of Klopp et al. and 4.5 to 10 kg mm-2 and 10-8 to 10-4 sec-1 for those of Gilbert et al., are overlapping. The activation energy for creep of our powder-metallurgy tungsten is 105,000 cal mole-1. This close agreement with the value found by Klopp et al. suggests that the same mechanism may be common to both types of materials. It may be possible to gain some additional insight into the rate-controlling mechanism by applying the analysis made by conrad22 in terms of the activation volume. The value for the activation volume depends upon the dislocation mechanism and may be used to help differentiate between various dislocation mechanisms. The activation volume for cross slip is 10 to 100 b3. Values determined from our data were 130 to 220 b3 which are in better agreement with the range of 102 to 104 b3 for nonconservative motion of jogs. Values determined from data of Klopp et al. are 240 to 1040 b3. We suggest that the rate-controlling mechanism for creep in this temperature range may be nonconservative motion of jogs assisted by enhanced diffusion along grain boundaries or dislocations. This model requires an activation energy lower than that for self-diffusion as is observed. If this is the controlling mechanism, a higher activation energy which is closer to that for self-diffusion might be expected for tests conducted on specimens with reduced grain boundary area, i.e., larger grain size. In support of this premise we have conducted tests on speci- mens having one to three grains per cross section for which a higher activation energy of 130,000 cal mole-1 was observed. Also, in agreement with results of Klopp et al., a faster creep rate resulted from the increased grain size and probable decreased dislocation density. Further argument against the cross slip mechanism is based on the constant activation energy we obsserved over the range of 5.0 to 10 kg mm-2,21 whereas the activation energy for cross slip displays a significant stress dependence.23 In addition to this, the powe on the stress term for the strain-rate dependence appears too high for cross slip. The values for tungsten fall in the range of 4.5 to 7 (Klopp et al. and Ref. 21) whereas values of approximately 2 are observed in creep by cross slip for hep metals.24 At temperatures from 3300° to 4000°F, Klopp et al. observed an activation energy of 141,000 ± 4000 cal mole-' which is less than that for self-diffusion, 153,000 cal mole-1, 25 and less than that reported for high-temperature creep of powder-metallurgy tungsten by Green:' 160,000 cal mole-1. Klopp et al. suggested that recovery of strain hardening by dislocation climb is the rate-controlling mechanism in this temperature region. Actually an activation energy larger than that for self-diffusion is predicted by this model if the temperature dependence of the elastic modulus27 is taken into consideration. Klopp et al. attributed this lack of correlation to the compositional differences between powder-metallurgy tungsten used by Green and their own arc- and EB-melted tungsten. It is our position that the value of 141,000 ± 4000 cal mole-' represents a transitional value between the higher and lower activation energies and does not represent a discrete mechanism of deformation. If the tests had been extended to higher temperatures the higher value of activation energy would have been observed as has been demonstrated by both our analy sis'' of isothermal test data by GE-NMPO28 and differential temperature tests28 on are-melted tungsten. The activation energies determined (170,000 and 160,000 cal mole-1) were greater than that for self-diffusion and are in better agreement with the value found by Green. The model of dislocation climb is associated with ; activation volume of 1 b3 according to Conrad.22 The activation volume calculated for the creep data of fou independent investigators in the temperature range where the activation energy for creep is near that for self-diffusion (Klopp et al. and Refs. 26, 28, and 30) is 110 to 2800 b3 and is in the range suggested for nonconservative motion of jogs. In the case of tungsten this mechanism may be preferred over that of dislocation climb. Sincere appreciation is expressed to Messrs. J. E. Flinn and F. L. Yaggee for the helpful discussions and suggestions in the preparation of this communication.

Jan 1, 1967

By W. P. Sykes

SINCE Honda and Murakami1 in 1918 proposed their constitutional diagram of the carbon-free iron-tungsten system, considerable effort has been expended by several investigators in attempts to define more positively the structural features of the alloys. The existence of an intermediate phase corresponding to the formula Fe3W2 (68.7 per cent W) was proposed from evidence of a purely metallographic nature by one of the present authors2 in 1926. Since that time the identity of this phase has been confirmed by Arnfelt3 and by Takeda,4 both of whom employed X-ray methods as well as the microscope and the chemical analysis of isolated microconstituents. According to Arnfelt, Fe3W2, as crystallized from the iron-rich melts at a temperature above 1450'C., contains by analysis 68.7 per cent W. The lattice of this phase is characterized by trigonal symmetry. Arnfelt, moreover, proposed a second intermediate phase formed at some temperature between 1450° and 1000° C. by a peritectoid reaction involving Fe3W2 and the iron-rich solid solution. A melt containing 25 per cent W was cooled to 1000° C. and heated for. 100 hr. The precipitated tungsten-rich constituent was separated and found by analysis to contain 62.6 per cent W. This composition agrees closely with that represented by the formula Fe2W (62.2 per cent W). Diffraction patterns from the concentrated precipitate showed a hexagonal unit cell. Takeda confirmed the data of Arnfelt regarding Fe3W2 but was unable to detect Arnfelt's second intermediate phase. While Takeda. failed to describe in detail the treatments employed, he stated that in alloys containing 40 per cent W which were quenched after heating at various temperatures between 1200° and 1450° C., no evidence of the second phase (Fe2W) was observed either in the microstructure or in the diffraction patterns of isolated residues. He therefore considered the existence of this low-temperature hexagonal compound as disproved.

Jan 1, 1932

By M. L. White, J. L. Shafer, C. L. Caenepeel

Often an in situ leach is the only practical economic method for copper recovery from small low grade oxide deposits. The decision to develop a copper property by an in situ blast and leach is strongly dependent on ore grade, tonnage, hydrology, and the copper extraction and acid consumption rates. The inherent leachability of the ore will in part determine the desired amount of fracturing of the ore deposit by the blast in order to obtain a copper extraction rate that is economical. For the last several years Occidental Research Corp. (ORC), has undertaken a modest effort to address the question of how to best identify and determine the information necessary to predict and control the operation of an in situ leach for the economic recovery of copper.

Jan 2, 1979

By A. R. Anderson

UNTIL recently all discussions directed at justify-ing the use of mechanical-loading equipment and conveyors have referred chiefly to tons per man and cost per ton. But there is another consideration that ? will speed the adoption of mechanical loading in mines even though tons per man on present day stand-ards were not increased nor the cost per ton decreased. With restricted immigration, improved facilities for education in our mining communities, and increased opportunities for recreation, the type of man who can or will throw 20 tons of coal per day over the side of a mine car is disappearing. Whether we will it or not provision must be made to replace muscular effort by mechanical means. Fortunately, indications are that the process will be accompanied by increased output per man and lower production cost, and though the outlook may now be a bit clouded in spots, all should profit by the change. The operator should enjoy a more stable business with more assured profit, the miners should get a better livelihood with less arduous effort and under safer and pleasanter working conditions, and the consumer should gain the assurance of a supply of coal always available at reasonable prices. That sounds like the millennium in the coal business perhaps. Of course, it is not, but there is just enough of that millennium stuff in it to encourage those of us who are working with today's problems of applying loading and conveying equipment to underground opera-tions. If we discern clearly that there can be no back-sliding, and that all will share in whatever advantages accrue, we will carry on more vigorously, and may right-fully expect to have the necessary cooperation of all the elements within the industry. As nature does not seem to have followed a definite plan in the formation of coal deposits it is not likely that any one standard method or type of equipment can be evolved for mining the coal. The method of mining that maybe most advantageously employed with load-ing machines and conveyors depends on the character of the strata overlying the coal as much as anything else.

Jan 4, 1927

By David V. Ragone, Richard E. Balzhiser

The liquidus uranium concentration in the U-Bi system is given by the following expression for the temperature range 400° to 800°C: No break was observed in the curve over this temperature range. The partial molar enthalpy change for uranium in the liquidus reaction, UBi2— U + 2Bi, was found to equal 12,300 cal per g mole. Copper produced a continuous decrease in the liguihs uranium concentration at 600°C. The presence of copper in the solvent was observed to affect the uranium activity coefficient according to the following expression: duced no change in the liquidus combosition below 0.6 at. pct Pd. Higher palladium concentrations sharply depressed the uranium concentration. SOLUTE behavior in molten alloys has been shown to be strongly influenced by the presence of additional species. Much attention has been given to such phenomena in iron-base systems where a number of alloying elements and/or impurities are likely to be present in small but significant quantities. Frequently, the interaction of these solutes has altered their thermodynamic behavior to the extent that reaction equilibra are appreciably influenced. Consequently, much of the information available for binary behavior must be reevaluated when additional components are likely to be present. Similar interactions can be expected to occur in bismuth-base solvents. Interest in the use of bismuth solutions of uranium as reactor fuels has stimulated investigators to explore the effect of various elements on the liquidus uranium concentration. Criticality requirements necessitate close control of the uranium concentration which, at the anticipated operating temperature of 500°C, approaches saturation. Consequently, elements which suppress the liquidus concentration could produce serious reactivity problems. Since the fuel solution is cer- tain to contain additives, such as magnesium and zirconium, for corrosion inhibition as well as small concentrations of fission products and corrosion products, a better understanding of the possible interaction phenomena is mandatory. This need stimulated experimental programs at the Brookhaven National Laboratory and elsewhere to determine precisely the liquidus uranium concentration in the bismuth-rich portion of several ternary systems. Early experimental efforts were directed toward an accurate dcmtermination of the U-Bi liquidus over the temperature range from 300' to 800°c. As shown in Fig. 1, the results to date exhibit considerable scatter. The investigations of Bareis,' Teitel,2 Greenwood,3 and Cotterill and hon4 agreed well below 700°c. Greenwood and Teitel extended their studies to higher temperatures but failed to concur in their results. A more recent study by Schweitzer and weekss at Brookhaven National Laboratory between 300' and 725°c, produced values 15 pct lower

Jan 1, 1962

By David Cole

At the time flotation appeared upon the metallurgical horizon in Arizona, the writer, under the direction of Dr. Ricketts, was engaged in remodeling and enlarging the No. 6 Concentration Plant of the Arizona Copper Co. at Morenci, and the work had been in progress nearly a year before the Inspiration experiments with flotation had disclosed the revolution in concentration that was at that time impending. The simplified flow sheet worked out for the remodeling of the Morenci plant had been based upon the removal of the freed metal in a minimum number of stages by treatment upon tables equipped with Butchart riffles, the latter being adapted to accomplish both classification of feed and removal of the metal at one operation, substantially as described in my previous paper.l The scheme of treatment for the slime was based upon the well-known fact that after copper sulphides, such as chalcocite and chalcopy-rite, etc., are reduced to a certain extremely fine state of comminution they are definitely beyond the reach of separation upon any of the concentrating devices then known. By using drag-belt classifiers (which served as conveyors as well as separators), the overflow ,would be of the usual "slimes" class. Experiment had shown that when these drag-belt overflows were properly diluted (that is, to about 5 to 7 per cent. solids in the feed under treatment) the very fine sand, and especially the very fine but still granular sulphide particles, would, if given a short distance to fall, quickly settle out in prime condition to yield an excellent recovery on vanners; a further valuable feature would be that the very fine non-separable final overflow tonnage might be discharged direct to tailing, thus conserving space requirements so as to permit within the old building, without embarrassment, the increase of capacity required. For reasons that are obvious, this kind of feed preparation for the slime could not be successfully accomplished in any form of pointed boxes or

Jan 1, 1917

Alfred Noble Joint Prize Committee F B Foley, '56 American Documentation Institute F B Foley, '56 American Geological Institute J L Gillson, Nov '56, H A Meyerhoff, Nov '57 Committee on Government Relations J L Gillson, '56 American Power Conference Paul R Nichols, '56 American Standards Association Mining Standards Board E R Borcherdt, Jan '58, Otto Herres, Jan '58 Alternates E W Bullard, Dec '56, and J K Richardson, Dec '56

Jan 1, 1956

By Terje Preber

Undisturbed sampling of shale has always been difficult. As pert of a comprehensive subsurface investigation for a nuclear power plant in northwestern Illinois, the Maquoketa shale, which contains seams of argillaceous dolomite, was sampled using different coring techniques. Since the Maquoketa shale is extremely fissile, careful sampling preservation by both lateral and vertical confining was utilized. The samples were tested to determine both static and dynamic properties. A relationship between void ratio and compression index, swell index, and swell pressure ratio was established. Correlation was found between the dynamic properties and both undrained shear strength and confining stress. Based on the results of the sampling and testing programs, recommendations for sampling and sample preservation techniques are given. INTRODUCTION Undisturbed sampling and preservation of samples of weathered, fiasile shale is often a very difficult task. The often erratically varying degree of weathering with depth complicates sampling and makes reproducibility of testing results difficult. Therefore, the testing of weak, weathered rock very often yields a wide variety of test results with large data scatter. The reproducibility of teat results usually associated with water-deposited soils is seldom, if ever, obtained. The testing and sampling program described in this paper was part of a comprehensive subsurface investigation for a nuclear power plant in northwestern Illinois. The sampling, preservation and testing program of shale samples taken from the Maquoketa shale are described, and, in particular, the different sampling techniques and sample preservation procedures are evaluated with respect to their effectiveness. The samples obtained by these procedures were subjected to a comprehensive testing program, including both static and dynamic testing in order to provide input for soil-structure interaction analysis. GEOLOGY The Maquoketa Shale Group is of Ordovician age and is part of the Cincinnatian Series. The area where the shale samples were taken was in a broad sea far from sources of clastic sediments during most of Ordovician time. However, during Cincinnatian time when large deltas in the Appalachian region were being formed, clastic sediments from the east dominated the sedimentation ii. Illinois, resulting in formation of the shale and dolomite shales of the Maquoketa Shale Group (Willman et al., 1975). The geologic unit sampled consists of a greenish gray to gray silty shale containing numerous 1- to 12-inch (2.5- to 30.5-cm) thick interbeds of argillaceous dolomite. The dolomite comprises up to 40 percent of the profile studied. The shale

Jan 1, 1984

By W. O. Hotchkiss

IN CONSIDERING the question of mining methods the possible rate of production deserves much more attention than it often receives. Hoover's theorem that, in order to show the greatest profit, an orebody should be worked out in the shortest practicable time, should be better known. The author recently' obtained detailed statements of costs from iron-mine superintendents of the Lake Superior district. In discussing these, the effect of rate of mining on cost of production was considered and detailed estimates were made. The methods by which these estimates were made and the way in which they were presented are here described to illustrate the importance of this factor in mining operations. The saving due to lower costs is not the only factor that should be considered. The greater profit per ton is of much importance but of equal importance are the greater profit per ton that will be made on a greater number of tons per year, and the fact that the total profit will be received in a shorter; period. This last makes a great difference in the present value of a property, by shortening the period of discount on future profits. Another item of importance to those operating a number of mines is that the tonnage needed to supply the market can be obtained most profitably by operating the smallest number of mines that will supply the amount required when each is worked to maximum capacity. In the Lake Superior iron district there are many grades of ore, and the requirements for each are known. If the demand for a certain grade can be supplied from mines now operating, the development and mining of a new orebody of the same grade must result in lower rates of production and lower profits to all mines producing this grade. If a company is mining the same grade of ore from three mines when it can supply its needs by operating only two, by operating only two it can obtain the greatest profit. Royalty rates, lease terms, and other considerations modify this general statement, but if all three properties

Jan 5, 1922

By Jesse O. Betterton

Recently some experimental work was conducted by the author in connection with the direct leaching of certain zinc ores with sulfuric acid with the object of subsequently recovering the zinc by electrolysis. The ores contained relatively large quantities of soluble silica, making it necessary to evolve special methods for handling the silicate solutions resulting from a leach of the ore, and also for the final removal of the silica before electrolysis. The problem was complicated by the presence of vanadium in the ore, the commercial recovery of which was very desirable. This paper, however, deals only with the silica phase of the problem. The zinc in the ore occurs in the form of a silicate (hemimorphite) and, to a very small extent, as the phosphate (hopeite) and carbonate (calamine); the vanadium is found as descloizite and vanadinite but mainly as descloizite. The experimental work was done in a plant producing 50 lb. of zinc = daily, in which the complete cycle of operations, including the final electrodeposition of the zinc, was performed continuously for one year. Some of the conclusions given here are the result of the operations in -this plant; the others are from laboratory tests inaugurated both as a guide to the plant operations and, in certain cases especially, to determine the limits in question. The practice in the 50-lb. zinc plant was to direct leach the ore crushed to pass 40 mesh, with spent electrolyte from the cells containing approximately 3 per cent. zinc and 10 per cent. free acid. This resulted in an acid leach solution and an ore residue. The acid leach solution was ' subjected to a special treatment for subsequent removal of vanadium; then the silica and vanadium in solution were precipitated together and removed as a "silica residue" by pressing through an ordinary plate and frame press. The next step was to treat the filtrate from the silica residue with zinc dust as a final purification step before it went to

Jan 1, 1923

By Jesse O. Betterton

Recently some experimental work was conducted by the author in connection with the direct leaching of certain zinc ores with sulfuric acid with the object of subsequently recovering the zinc by electrolysis. The ores contained relatively large quantities of soluble silica, making it necessary to evolve special methods for handling the silicate solutions resulting from a leach of the ore, and also for the final removal of the silica before electrolysis. The problem was complicated by the presence of vanadium in the ore, the commercial recovery of which was very desirable. This paper, however, deals only with the silica phase of the problem. The zinc in the ore occurs in the form of a silicate (hemimorphite) and, to a very small extent, as the phosphate (hopeite) and carbonate (calamine); the vanadium is found as descloizite and vanadinite but mainly as descloizite. The experimental work was done in a plant producing 50 lb. of zinc = daily, in which the complete cycle of operations, including the final electrodeposition of the zinc, was performed continuously for one year. Some of the conclusions given here are the result of the operations in -this plant; the others are from laboratory tests inaugurated both as a guide to the plant operations and, in certain cases especially, to determine the limits in question. The practice in the 50-lb. zinc plant was to direct leach the ore crushed to pass 40 mesh, with spent electrolyte from the cells containing approximately 3 per cent. zinc and 10 per cent. free acid. This resulted in an acid leach solution and an ore residue. The acid leach solution was ' subjected to a special treatment for subsequent removal of vanadium; then the silica and vanadium in solution were precipitated together and removed as a "silica residue" by pressing through an ordinary plate and frame press. The next step was to treat the filtrate from the silica residue with zinc dust as a final purification step before it went to

Jan 1, 1923

By H. S. Strouth

JAMAICA-bauxite and gypsum-but what else? J Does the Caribbean island have anything more to offer in the form of mineral wealth? One answer may be iron ore deposits which show enough promise to warrant exploitation in the near future by a company associated with Standard Ore & Alloys Corp. In addition, Jamaica is reported to have gold, silver, platinum, copper, lead, zinc, manganese, cobalt, and a great many nonmetallic minerals. Of these, only platinum has not been produced commercially in the past. Right now, Jamaican bauxite is getting most of the publicity, but not too long ago other mining operations were in progress. Lack of proper interest, insufficient roads, and scarcity of venture capital forced those mining properties to suspend production.

Jan 7, 1954

By H. L. Miaw, A. M. Gaudin, D. W. Fuerstenau

IN spite of considerable study,1-5 the nature of slime coatings in flotation is still not completely understood. However, phenomena that control flocculation and dispersion of colloidal systems are now interpreted in terms of electrical double layers."' Colloids will flocculate even though the particles carry the same charge, but when two dispersed colloids of opposite charge are mixed, flocculation ensues even more rapidly. Analogous phenomena seem responsible for slime coating on minerals in flotation systems. To shed new light on the issue it was considered desirable to devise a tool that would measure slime coatings. The usual method has been to examine photographs of presumably representative surfaces, after an intervening washing in running water. But such an examination is non-quantitative, and the changes in chemical environment represented by the washing may have removed the slime coatings that existed during flotation. To provide the possibility for a correlation with electrical double layer phenomena, the experiments were made with quartz, corundum, and iron oxide, for which electrokinetic data are available.8-12 Since the properties of the electrical double layers of these oxides depend on the pH of the solution, pH will be the most important variable. Furthermore, because the zero point of charge for silica, iron oxide, and alumina occurs at pH 3.7, 8, and 9.5, respectively, the relative charge on the slime and mineral can be changed over wide ranges. Because of its practical importance in quartz flotation, iron oxide powder was chosen as the slime. Also, its uniform composition, contrasting color, and ease of analysis make experimentation simple.

Jan 7, 1958

By R. J. Walter, W. T. Chandler

The Ch-H phase diagram was determined for by-drogen concentrations up to ChHo.9 at temperatures below 400°P'. The phase diagram includes a mis-cibility gap and a eutectoid transformation. A peri-tectoid transformation is postulated at the hydrogen-rich end of the diagram, Phase diagrams were determined for two levels oj purity, of the columbium. A single solid solution exists in the Cb-H system above 400°F. There has been considcrable disagreement among investigators concerning the system at temperatures below 400°F. Albrecht, Goode, and ~allett' proposed a miscibility gap containing two bcc phases with the two lattice parameters converging at about 140°C (285-F), and Brauer and ~erman' found a two-phase room-temperature region between 10 and 41 at. pct H. At sufficiently high hydrogen concentrations in the one-phase region, the hydrogen-rich phase was found to be face-centered orthorhombic. Wainwright, Cook, and Hopkills3 recently reported that the face centered orthorhombic hydride phase is derived from a unit cell which is slightly tetragonal with a small departure from 90 deg of the angle (y) opposite the r axis. The orthorhombic hydride phase was observed for hydrogen concentrations between 0.2 and 0.8 H/Cb atom ratio. Paxton and coworkers4 found that needlelike hydride plates formed in a hydrogen-charged columbium single crystal and suggested that this transformation possessed the characteristics of a diffusionless phase transformation. On the basis of room-temperature, X-ray diffraction data, komjathy' suggested that an order-disorder or martensitic transformation occurs. In the present study, the Cb-H system was investigated to resolve the discrepancies found in the literature for this system. PROCEDURE The columbium specimens were prepared from two heats of wrought 1/2-in.-diameter electron-beam melted columbium rod and from two columbium powders of -80 mesh size of different impurity contents. The columbium bar stock was pur chased from Urah Chmg Corp.; the 99 and 99.5 pct purity colulnbium powders were obtained from Fansteel Metallurgical Corp. and Kern Chemical Co.. respectively. The chemical analyses of the columbium bar and powders are listed in Table I. Hydrogen charging was performed by exposing the columbium specimens to hydrogen at 1 atm pressure at various temperatures. After exposure the specimens were quenched to prevent the hydrogen pickup which would take place if cooled in hydrogen, or the hydrogen loss that would occur if cooled in an inert gas. Adequate hydrogen purity was achieved by passing high-purity tank hydrogen (maximum 5 ppm total impurities) through an Engelhard catalytic Deoxo unit, magnesium per chlorate desiccant, and finally through activated charcoal at the temperature of boiling nitrogen. Activated charcoal at -321°F has been reported6 to remove impurities from hydrogen to a nondetectable level. A schematic representation of the heat-treating apparatus is shown in Fig. 1. A metal-sheathed thermocouple embedded in the colun~bium specimen was used to control the temperature during heat treatment and to pull the specimen boat into

Jan 1, 1965

By John P. Goheen

Considerable work has been done in developing a pyrometer to measure the temperature of molten brasses, bronzes, and aluminum in the crucible. On account of the high melting points and the amount of zinc and sulfurous fumes given off from molten brasses, the conditions are somewhat severe for a thermocouple of standard design; but satisfactory results are obtained with a portable pyrometer, 3 ft. (0.9 m.) of connecting lead wire, and a special 5-ft. nickel-nickel chromium thermocouple, composed of rods 1/4in. (6.35 mm.) in diameter. The lower 12 or 24 in., as desired, may be made detachable so that new tips may be connected at little trouble or expense. The portable instrument need not be of the extreme high-resistance type, as the movable parts of the galvanometer of a lower resistance instrument may be better constxucted to withstand the continuous handling such an instrument receives. Platinum-platinum rhodium thermocouples, protected with porcelain and graphite tubes, have been used, but the lag in registering the temperature is too great. It has been found that the range of temperature for various brasses is as follows: Red brasses...............2200-2250" F. (1205-1234" C.) Yellow brasses............2250-2400" F. (1234-1318' C.) Bronzes..................2300-2550" F. (1260-1400" C.) A recent test with a portable pyrometer having a range of 2600" F. with a bare 1/4 in. heavy exposed couple 5 it. long and a handle attached at the upper end showed that the temperatures of molten aluminum under varying conditions in an oil-fired crucible furnace and one of the Simplex type were as follows: CRUCIBLE, OIL-FIRED FURNACE SIMPLEX FURNACE Temperature of metal in furnace....... 1540" F. (837" C.) 1530" F. (834" C.) Temperature in ladle after skimming at furnace......................... 1480" F. (805" C.) 1440" F. (784" C.) Temperature in ladle after skimming at floor near mold................... 1440" F. (784" C.) 1430' F. (778" C.)

Jan 1, 1923

By John P. Goheen

Considerable work has been done in developing a pyrometer to measure the temperature of molten brasses, bronzes, and aluminum in the crucible. On account of the high melting points and the amount of zinc and sulfurous fumes given off from molten brasses, the conditions are somewhat severe for a thermocouple of standard design; but satisfactory results are obtained with a portable pyrometer, 3 ft. (0.9 m.) of connecting lead wire, and a special 5-ft. nickel-nickel chromium thermocouple, composed of rods 1/4in. (6.35 mm.) in diameter. The lower 12 or 24 in., as desired, may be made detachable so that new tips may be connected at little trouble or expense. The portable instrument need not be of the extreme high-resistance type, as the movable parts of the galvanometer of a lower resistance instrument may be better constxucted to withstand the continuous handling such an instrument receives. Platinum-platinum rhodium thermocouples, protected with porcelain and graphite tubes, have been used, but the lag in registering the temperature is too great. It has been found that the range of temperature for various brasses is as follows: Red brasses...............2200-2250" F. (1205-1234" C.) Yellow brasses............2250-2400" F. (1234-1318' C.) Bronzes..................2300-2550" F. (1260-1400" C.) A recent test with a portable pyrometer having a range of 2600" F. with a bare 1/4 in. heavy exposed couple 5 it. long and a handle attached at the upper end showed that the temperatures of molten aluminum under varying conditions in an oil-fired crucible furnace and one of the Simplex type were as follows: CRUCIBLE, OIL-FIRED FURNACE SIMPLEX FURNACE Temperature of metal in furnace....... 1540" F. (837" C.) 1530" F. (834" C.) Temperature in ladle after skimming at furnace......................... 1480" F. (805" C.) 1440" F. (784" C.) Temperature in ladle after skimming at floor near mold................... 1440" F. (784" C.) 1430' F. (778" C.)

Jan 1, 1923

By P. A. Fisher, J. B. Wilson, D. J. Whitehead, C. J. P. Ball, A. C. Jessup

The properties of a new magnesium alloy ZT1 containing 3.0 pct Th, 2.5 pct Zn, 0.7 pct Zr are described. The alloy possesses good creep and fatigue resistance up to 650°F, is free from microporosity, and is readily sand-cast. ZT1 is shown to be superior to zinc-free Mg-Th-Zr alloys. THE advent of the jet engine created a demand for a light sand-casting alloy capable of being cast into large complex shapes and capable of resisting creep at temperatures up to 500°F. This demand has been largely met by alloys of the magnesium-cerium mischmetal-zirconium types, containing about 3 pct Ce mischmetal and 0.7 pct Zr, typified by Elektron magnesium alloys MCZ and ZREI, the latter alloy also having a zinc addition of 2.5 pct. These alloys utilize the valuable properties at elevated temperatures conferred by the addition of rare earth metals to magnesium, a fact which has been known for many years and discussed by several investigators.1-1 Murphy and Payne8 showed that the addition of the powerful grain-refining element zirconium to Mg-Ce mischmetal alloys produced alloys with attractive room temperature properties combined with good creep properties and castability. With the increasing power of modern jet engines the temperatures to which some of the magnesium parts are subject are likely to exceed the safe working range of the cerium-mischmetal-containing alloys, and at the beginning of the research considerable interest had been shown by aeroplane engine designers in a magnesium sand-casting alloy suitable for service at higher temperatures, e.g., 600°F and above. At an early stage in the development of this type of alloy a check on the fatigue properties at elevated temperatures indicated that, since the fatigue limit even at 108 eversals was appreciably higher than any permissible creep stress, the main emphasis of the research could be concentrated on creep behavior. The primary aim in developing the new alloy has therefore been to attain maximum creep resistance; but due consideration has also been given to other important properties such as castability, tensile strength, and cost. It is by now well established that it is not possible to correlate creep strength with other short time mechanical properties such as are obtained in tensile

Jan 1, 1954