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By D. R. Packard, J. D. Verhoeven

The resistivity us atom fraction relationships for dilute solutions of cadmium, mercury, and tin in molten sodium have been determined. With these data and the resistivity capillary-reservoir technique, the electro-transport mobilities, effective valences, and the diflusion coefficients of the three solutes have been determined. The mobilities are found to be higher than in other molten alloys by a factor of around 20. The results are compared to the Mmgelsdorf model for electrotrmtsport. The high values found for the mobility to diffusion coefficient ratio indicate that small quantities of the alkali metals should be susceptible to purification from many solutes by means of electrotransport. PASSAGE of a direct electric current through a liquid metal containing a solute will usually cause a relative motion between the solute and solvent atoms of the alloy. This electrotransport phenomenon may be described experimentally in terms of the mobility of the solute atoms, i.e., the drift velocity of the solute relative to the solvent per unit electric field. In dilute solutions of liquid alloys this relative mobility becomes a measure of the velocity of the solute with respect to the observer since the motion of the solvent is negligible. The mobility is a significant parameter in evaluating the potential usefulness of electrotransport for such things as purification or solute control upon solidification. Prior to around 1958, quantitative data for the mobility of solutes in liquid metals were restricted to some solutes in liquid mercury. Since that time ad- ditional data have been reported for the mobility of solutes in liquid mercury, bismuth, tin, and lead, as shown in Table I. In 1963 Drakin et al.11 reported some values of a transport number for mercury and thallium in molten sodium and potassium. When these values were converted to mobilities, it was found that the mobilities were higher than any of the previously reported values by a factor of around 20, as shown in Table I. Drakin's experimental technique did not eliminate the presence of back-diffusion and consequently his data were expected to be lower than the true values. The purpose of the present investigation was to determine the mobility of a number of solutes in molten sodium with an experimental technique which eliminates back-diffusion errors. EXPERIMENTAL The technique used to determine the mobility was a resistivity capillary-reservoir technique which had previously been used with a high degree of precision on Sn-Bi alloys.4 This technique consists of dipping the vertical Pyrex capillary cell shown in Fig. 1 into a molten bath of alloy while the bath and capillary are under vacuum. The capillary is then filled by intro-

Jan 1, 1969

By F. D. Rosi

The plastic properties of extended silver and copper crystals of varying purity were studied as a function of crystal orientation in the early stages of flow. Variations in the gross shape of the shear stress-shear diagram and in the properties of critical Variationsshear stress and shear-hardening coefficient were correlated with changes in slip-band developments. The phenomenon of work hardening is discussed in terms of the existing dislocation theory. IT appears certain from the early studies on the deformation characteristics in metal crystals1-3 that plastic flow takes place in a preferred crystallo-graphic slip system which is determined by the geometry of the crystal (law of maximum shear stress), and that the value of shear stress for this system is independent of crystal orientation (law of critical shear stress). Experimentally, it has been demonstrated further that the law of critical shear stress can be extended to include extensive plastic flow.&apos; Thus, the shear-hardening coefficient, which is defined as the slope of the shear stress-shear curve, also is considered to be independent of orientation. It is noteworthy that deviations from this empirical shear-hardening law have been reported in cubic crystals whose initial orientation favors slip on more than two systems.&apos; Moreover, this law appears to have been derived from stress-strain data relating to relatively high values of shear strain (0.5 to 4), where widespread slip and complex distortions can be expected, regardless of crystal orientation. Since existing data indicate that the strain inhomogeneity in a crystal is manifested particularly in the early stages of flow, it would appear that a more exacting test as to the fundamental nature of the shear-hardening law would be to investigate systematically the shape of the stress-strain curve as a function of crystal orientation in the earlier stages of deformation. With regard to the general form of the shear stress-shear curve for cubic crystals, early studies show a parabolic hardening law, where the shear 1 stress is proportional to the square root of the shear-strain. Since this law was predicted theoretically by Taylor" in his original dislocation model for hard- ening, it has been accepted widely as a fundamental flow characteristic of cubic metals. However, it was recently pointed out by Masing6 hat the parabolic law is not the elementary form of hardening in cubic crystals, but instead is a consequence of complexities in the flow process (e. g., deformation bands and unpredicted secondary slip). Thus, in the very early stages of deformation (< 2 pct extension) where the occurrence of such complexities is unlikely, a different strain-hardening behavior might be anticipated. This view is supported by the recent work of Rosi and Mathewson7 on high purity aluminum where a linear law was obtained for extensions up to 2 pct. A linear hardening over a wider range of deformation also was reported by Rohm and Kochendorfer8 ho deformed aluminum crystals under conditions approximating pure shear. Even more pertinent is the recent evidence of Masing and Raffelsieper9 on high purity aluminum crystals. It was found that for crystals having initial orientations near a <l00> or <1ll> axis, a high hardening was obtained, whereas crystals with a <110> orientation exhibited a low and linear hardening curve followed by a region of more rapid hardening. Since much still remains obscure concerning the details of strain hardening as well as slip-band formation in face-centered-cubic crystals in the early stages of deformation, the present study was undertaken to evaluate the effect of crystal orientation on these two important manifestations of glide. It is important to note here that at the time of this study, Lucke and Lange11 presented information on the orientation-dependence of the shape of the strain-hardening curve in aluminum of various purities. Their work, which essentially represents an extension of that of Masing and Raffelsieper, in many respects is parallel to that of the present study. Experimental Procedure Production of Single Crystals: Single crystals of silver and copper of varying purity were used in

Jan 1, 1955

By P. K. Koh, G. C. Dunn

Si-Fe single crystals in a number of selected orientations were cold rolled 70 pct and analyzed to obtain quantitative (110) pole figures. Stable end orientations were ddetermined, and the effect of orientation on deformation behavior was investigated. WHEN single crystals are cold rolled sufficiently, they rotate into end orientations that are stable or unchanged in position with additional deformation. The end orientations of heavily cold-rolled iron crystals, positioned in holes in copper to limit lateral flow and to simulate polycrystalline conditions during deformation, were determined by Barrett and Levenson.&apos; They found that the sum of the end orientations, a pole figure for all the crystals studied, reproduced the essential features of the cold-rolled texture of polycrystalline iron. In. an investigation of Fe-Si alloys, Barrett, Ansel, and Mehl&apos; observed little effect of silicon content on the textures of heavily cold-rolled samples. Since alloys with less than 4 pct Si are known to have the same slip systems as iron," it seems logical to expect that they would also have the same end orientations as those for iron. Whereas Barrett and Levenson in their study of single crystals were interested in the problem of the origin of the cold-rolled texture of polycrystalline iron, the present authors are more interested in the final cold-rolled textures of single crystals of Si-Fe from the point of view of their relationship to subsequent recrystallization phenomena which will be reported in another paper. Nevertheless, such points as the tendency of an end orientation not to rotate (stability), the tendency of a pole concentration to spread out, and the tendency of the crystal to widen during cold rolling become interesting separately when the initial orientations are selected already in end orientations. Also the initial orientations having a [I101 axis parallel with the transverse direction, which include the two end orientations (111) [Ti21 and (001) [110], comprise a series that needs further clarification regarding the way such crystals rotate during deformation. Finally the present use of quantitative pole figure methods* represents an advance over the X-ray photographic method employed by Barrett and Levenson in their work on end orientations. The present investigation provides information on the cold-rolling behavior of two groups of Si-Fe crystals: 1-—crystals initially oriented in recognized end orientations for iron crystals with a [I101 direction parallel with the rolling direction, and 2— crystals initially oriented with a [I101 direction 90" to the rolling direction and in the rolling plane. For the second group, there is a 90" range between the (001) [110] orientation and the (110) [001] orientation. Since the 35" portion of this range from (110) [OOl] to (111) Di2] was included in a previous investigation," only the remaining 55" portion from (111) fii2] to (001) [I101 needs further consideration. Also, since both (111) [xi21 and (001) [I101 are end orientations for iron crystals,&apos; there might be a critical orientation* or orientation range be- • W. W. Martin and C. G. Dunno noted that (112) [Till was such a critical orientation. tween them such that early in the deformation an orientation within this critical range splits into two orientations. Upon further deformation, these two orientations rotate to produce a final texture consisting of (001) [1101 and (111) [?i2] components. The end orientations obtained are discussed in connection with the work of Barrett and Levenson, while the observed tendency for lateral flow of crystals in these orientations is treated in terms of the theory of Hibbard and Yen.&apos; Lateral flow according to the theory increases with deviation of the plane containing the rolling direction and the slip direction from a position perpendicular to the plane of rolling. Experimental Procedure Single crystals in sheet form with preselected orientations were prepared by methods that have been described elsewhere." Three lots designated A, B,

Jan 1, 1956

By F. D. Rosi, C. A. Dube, B. H. Alexander

WHEN a deformed polpcrystalline metal is heated to a sufficiently high temperature, a recrystallized structure develops which consists of small, essentially stress-free grains. This transformation is referred to as primary recrystallization. Under certain conditions, on prolonged annealing of the specimens, a type of grain coarsening occurs in which a small number of grains commence to grow at various points by devouring the neighboring finegrained primary structure, which, in itself, exhibits a marked stability toward normal grain growth. This grain coarsening process has been referred to by Burgers&apos; as "secondary recrystallization" or "exaggerated grain growth." Although much work has been done on recrystallization and growth processes, present knowledge of the factors which determine the occurrence and growth of secondary grains is inadequate for the advancement of a theory which accounts for the observed characteristics of this recrystallization phenomenon. In this respect, it would be important to make measurements of the velocity of growth of these large secondary grains. The early work of Feitnecht2 on aluminum showed that the size of secondary grains increased with temperature and time, suggesting that such measurements would be possible. More recently, Burgers1 found that the growth velocity of these grains in aluminum was constant over a large time interval, as is generally found for the growth velocity of primary grains in a uniformly deformed test piece.3-5 It is reasonable to expect that the determination of the activation energy of the secondary growth process might lead to a better understanding of the underlying atomic mechanism. This investigation, therefore, is one of a series primarily designed to measure the growth velocity of secondary grains at various temperatures for silver, copper, and aluminum. It is hoped that these studies along with those of orientation relationships, will establish a sound basis for theorizing as to the origin and nature of the secondary transformation. Experimental Procedure The metal used in the present investigation was high-purity silver (999.9 fine), which was supplied in the form of cold-rolled plates 0.250 in. thick. These plates were annealed at 500°C for 1 hr and then straight-rolled to a thickness of 0.04 in. in three reductions of approximately 45 pct, followed in each case by an anneal at 450°C for 1/2 hr. The 0.04 in. sheets were given a final reduction of approximately 50 pct, which resulted in a thickness of 0.02 in., thereby insuring two-dimensional crystal growth. Individual specimens of this material about 1x3 cm were used for all heat treatments, unless otherwise noted. The annealing was carried out under an atmosphere of argon in an Inconel tube furnace whose temperature was controlled to within -+2°C. Metallographic examination of the secondary transformation was accomplished by mechanically polishing the specimens on one side to approximately one half their thickness through 2/0 metallographic emery paper, and then electrolytically polishing in a solution of potassium ferrocyanide and sodium cyanide. With a current density of approximately 20 amp per sq dm, the time required to obtain a satisfactory surface varied from 3 to 5 min. Standard potassium bichromate was used to etch the electrolytically polished surfaces. A heavy etch with this solution produced a sharp contrast between the secondary grains and the fine-grained primary structure, darkening the latter while leaving the large secondary grains bright. All area measurements of the secondary crystals were made with a planimeter on enlarged tracings of the grains.

Jan 1, 1953

By A. R. Denison

Several productive areas in the Mid-Con-tinent are broadly and briefly examined with respect to the present depth of drilling on productive structures, and the thickness of sediments remaining untested. Evidence is offered to show that a vertical mile to two miles of untested but prospective formation remain within reach of the drill. In no case would a well deeper than 15,000 ft. be required, and in most cases to no greater depth than 10,000 ft. Recent outstanding success of deeper prospecting in West Texas demonstrates the merits of deeper drilling on known structure. Introduction New fields discoverd during I942 equaled or exceeded the number in any preceding year. The total amount of oil found by these discoveries was less than in any previous year, for which accurate records are available. This means that the pools now being discovered are much smaller than in past years. This is to be expected, since the prospects available during 1942 were largely those overlooked in the earlier years and therefore represent a second or third order (in quality) of structural feature. This failure to find pools of good size and quality raises grave doubt as to the security of our future oil supply. With military needs rising almost daily, and the period of heaviest con- sumption in our war effort still in the future, there is even a growing doubt as to our ability to supply the amount needed for our ultimate victory. This does not mean that our reserves are inadequate, but rather that our "capacity to produce" may be inadequate. Lacking large fields with flush production, our capacity to produce is rapidly approaching our current needs. ,Since the industry is unable to find the large new fields necessary to keep a safe margin of "capacity to produce," other means are needed. It seems obvious that one of these should be deeper prospecting on the large, proven, productive structural features now known. The exploratory wildcat is drilled primarily in search of a trap and the reason for failure to find oil and gas in nine out of ten cases is due to the absence of a suitable trap under the drill site. Therefore, deeper drilling on a known structural feature that is productive largely eliminates the greatest hazard in wildcat drilling. While by no means all the oil known today is found in structural traps—in fact, some have estimated that less than half is so located— the fact remains that structural traps are far more commonly the oil fields that have multiple horizons of production superimposed one over the other. Outstanding examples are the Eldorado field in Kansas, the Tonkawa and Cushing fields in Oklahoma, the Louden and Salem pools of Illinois, and the richest and most prolific of all structural traps, the Long Beach, Ven-tura and other similar fields of California.

Jan 1, 1944

By D. B. Masson

THE martensitic transformations occurring in ,B AgCd as a result of cold working at room temp.. a-ture and cooling below room ten1erature have been reported by Masson and Barrett.1 These authors found that simple cooling to 127°K caused body-cen-tered-cubic AgCd containing 53.0 at. pct Ag to transform to an orthorhombic structure, while mechanical deformation at room temperature was found to induce a hexagonal structure. Furthermore, they observed that the temperature at which martensite first appeared on cooling, Ms, and that at which the transformation was complete, MI, as well as the corresponding temperatures for the reversion on heating, As and Af, could be ascertained to ± 1°K, although they report these temperatures only for the alloy containing 53.0 at. pct Ag (51.96 wt pct). In the work reported here the temperature range of the transformation on cooling was studied as a function of composition, and further consideration was given to the relationship between the original bcc structure and the transformation-induced hexagonal and orthorhomic structures. EXPERIMENTAL PROCEDURE All samples studied were in the form of annealed 300-mesh powder and were prepared from the constituent metals in the manner described previously.1 The compositions in weight and atomic pct are listed in Columns 1 and 2 of Table I. Method of determination of transformation temperature was the same as utilized previously1—measurement of the intensity of X-rays diffracted by the transformation product. A diagram of the low-temperature sample mount is shown in Fig. 1. This mount was made to fit a GE model XRD-3 X-ray diffraction unit. The powder sample was varnished to a flat surface on a copper sample holder at A. This sample holder was soldered to a brass rod, B, which was in turn soldered to a second copper rod, C. Rod C could be cooled to 78°K by inserting it into a reservoir of liquid nitrogen, D. A heater coil of nichrome wire was wound at E on the sample holder, and by varying the current through the heater a thermal gradient could be maintained along brass rod B. Sample temperatures from 78°K up could be attained and held as long as needed. The sample holder and nitrogen reservoir were insulated by Styrofoam, F, and the sample itself was protected by two radiation shields, G. The X-ray beam entered and left the sample chamber through windoys in the supporting container at H and I. Sample temperatures were measured by a calibrated copper-constantan thermocouple varnished to the sample holder just out of the beam at A. The low-temperature structure had been found to possess orthorhombic symmetry1 and the expected positions of the diffraction maxima were known. Therefore the sample was aligned in the X-ray beam and the Geiger counter of the spectrometer set to receive the most intense orthorhombic reflection without an adjacent interfering cubic reflection. This

Jan 1, 1961

By A. R. Denison

Several productive areas in the Mid-Con-tinent are broadly and briefly examined with respect to the present depth of drilling on productive structures, and the thickness of sediments remaining untested. Evidence is offered to show that a vertical mile to two miles of untested but prospective formation remain within reach of the drill. In no case would a well deeper than 15,000 ft. be required, and in most cases to no greater depth than 10,000 ft. Recent outstanding success of deeper prospecting in West Texas demonstrates the merits of deeper drilling on known structure. Introduction New fields discoverd during I942 equaled or exceeded the number in any preceding year. The total amount of oil found by these discoveries was less than in any previous year, for which accurate records are available. This means that the pools now being discovered are much smaller than in past years. This is to be expected, since the prospects available during 1942 were largely those overlooked in the earlier years and therefore represent a second or third order (in quality) of structural feature. This failure to find pools of good size and quality raises grave doubt as to the security of our future oil supply. With military needs rising almost daily, and the period of heaviest con- sumption in our war effort still in the future, there is even a growing doubt as to our ability to supply the amount needed for our ultimate victory. This does not mean that our reserves are inadequate, but rather that our "capacity to produce" may be inadequate. Lacking large fields with flush production, our capacity to produce is rapidly approaching our current needs. ,Since the industry is unable to find the large new fields necessary to keep a safe margin of "capacity to produce," other means are needed. It seems obvious that one of these should be deeper prospecting on the large, proven, productive structural features now known. The exploratory wildcat is drilled primarily in search of a trap and the reason for failure to find oil and gas in nine out of ten cases is due to the absence of a suitable trap under the drill site. Therefore, deeper drilling on a known structural feature that is productive largely eliminates the greatest hazard in wildcat drilling. While by no means all the oil known today is found in structural traps—in fact, some have estimated that less than half is so located— the fact remains that structural traps are far more commonly the oil fields that have multiple horizons of production superimposed one over the other. Outstanding examples are the Eldorado field in Kansas, the Tonkawa and Cushing fields in Oklahoma, the Louden and Salem pools of Illinois, and the richest and most prolific of all structural traps, the Long Beach, Ven-tura and other similar fields of California.

Jan 1, 1944

By Walter Miller

A surprising development during the year was the continued high demand for petroleum products and the high level of crude oil charges to the stills. Generally speaking, the petroleum industry during 1946 succeeded in producing a greater quantity of crude oil and petroleum products than in any of the war years, and considerably exceeded the production of any prewar year. Daily crude still charges averaged between 4,700,000 and 4,800,000 bbl per day for 1946 and about equaled the 1945 record, although most pessimistic 1945 guesses, predictions, or fears ranged, for 1946, from only 3,900,000 to 4,400,000 bbl per day. In spite of the high crude charge to the stills, total stock of crude oil was higher at the end of the year by some 7,000,000 to 8,000,000 bbl. A similar story holds regarding stocks of the principal refined products. Gasoline on hand at year&apos;s end was two to three million barrels lower, and was considered low for the expected demand during the coming high consuming season, while stocks of light and heavy fuel oils, although some higher than a year previous, hardly reached a comfortable level. The trend in gasoline of high octane number, which has resulted in a marked rise in. the antiknock quality by the end of 1945 (five or six numbers higher than during the war and one number higher than the prewar quality of civilian motor gasoline of 1941) was abruptly arrested by an acute shortage of metallic lead for manufacturing tetraethyl lead. Government action in the form of lead price control, rationing, and the setting of octane ceiling specifications to conform to the reduced ethyl lead compound available were enforced until abrogated at the end of the year. It will be interesting to see how rapidly the octane levels will resume the rising trend, as more metallic lead slowly becomes available for making greater quantities of ethyl lead compound. As octane quality rises over present levels the disadvantage of the refiner without catalytic cracking equipment will increase. Gasoline made by catalytic cracking, without addition of ethyl lead, approximates 77 octane by the official ASTM Motor Method test, compared with 66 for gasoline generally similar in volatility made by the older thermal cracking operation. Catalytic gasoline shows an even greater improvement in the Research octane number, the comparison being roughly 86 Research versus 71 Research octane for the thermal cracked product. This higher differential in Research octane is credited by many, although not universally so, as contributing to better road performance, and consequently resulting in a more desirable product marketwise. In some parts of the country a premium of roughly one fourth cent per gallon is now being paid for gasoline with higher Research octane made possible by including catalytic cracked product in the final blends. If such price differentials in favor of catalytic gaso-

Jan 1, 1947

By E. DeGolyer

The problem of good engineering practice and. of good conservation practice in oil production is that of keeping gas in solution. This can best be done by producing a field as a water-drive field. Some degree of water drive is believed to be present in most fields but in the past most fields have been produced too rapidly to allow water drive to be effective. Ultimate recovery should be So per cent greater for fields produced by water drive over that from gas-expansion fields. Wide spacing will permit fields of low-degree water drive to be produced effectively as water-drive fields. INTRODUCTION NEGLECTING all the complicated scientific and technical argument that leads to the conclusion, the solution of the problem of good production practice, of good engineering practice, and of good conservation practice in oil production is to keep gas in solution. This can best be done by producing fields at a rate low enough to make effective the water drive, which exists, it is generally believed, to a degree great enough to be made effective in more than 80 per cent of the fields of the United States. Oil is being so produced in the Ten Section field of California; the Hobbs field of New Mexico; the Yates, Hastings, Friendswood, Anahuac fields and the main sand of the Conroe pool, in Texas; the Magnolia pool in Arkansas, and doubtless in many other pools. The measures of success in the efforts to achieve the solution of the problem are the maintenance of bottom-hole pressure and the prevention of an increase in gas-oil ratio. Some decline from the original bottom-hole pressure and the production of some gas are essential. A pressure gradient from the reservoir to the well is necessary and at least as much gas must be produced as that in solution in a barrel of oil. Once the optimum pressure and the gas-oil ratio have been established, they should be maintained. How common is water drive in oil and gas pools? General opinion is that some degree of water drive is almost universal. Theoretically, this conclusion appears to be a sound one. According to our present understanding of the processes of sedimentation, we would expect to find all sands or sandstone charged with connate water unless it had been displaced by some other fluid, such as fresh water percolating into the beds at the outcrop, or oil and gas, or gas only, in reservoirs. The fact that the original pressure of the fluid system in most reservoirs is approximately that of the hydrostatic head of water for the corresponding depth indicates that the sands are charged with water, and common experience in drilling into the extensions of the porous zones beyond the reservoir is to find them watercharged. The very fact that oil and gas pools have substantial pressures in their original undisturbed state indicates either that a reservoir is a rigid, closed system, a con-

Jan 1, 1941

By Walter Miller

A surprising development during the year was the continued high demand for petroleum products and the high level of crude oil charges to the stills. Generally speaking, the petroleum industry during 1946 succeeded in producing a greater quantity of crude oil and petroleum products than in any of the war years, and considerably exceeded the production of any prewar year. Daily crude still charges averaged between 4,700,000 and 4,800,000 bbl per day for 1946 and about equaled the 1945 record, although most pessimistic 1945 guesses, predictions, or fears ranged, for 1946, from only 3,900,000 to 4,400,000 bbl per day. In spite of the high crude charge to the stills, total stock of crude oil was higher at the end of the year by some 7,000,000 to 8,000,000 bbl. A similar story holds regarding stocks of the principal refined products. Gasoline on hand at year&apos;s end was two to three million barrels lower, and was considered low for the expected demand during the coming high consuming season, while stocks of light and heavy fuel oils, although some higher than a year previous, hardly reached a comfortable level. The trend in gasoline of high octane number, which has resulted in a marked rise in. the antiknock quality by the end of 1945 (five or six numbers higher than during the war and one number higher than the prewar quality of civilian motor gasoline of 1941) was abruptly arrested by an acute shortage of metallic lead for manufacturing tetraethyl lead. Government action in the form of lead price control, rationing, and the setting of octane ceiling specifications to conform to the reduced ethyl lead compound available were enforced until abrogated at the end of the year. It will be interesting to see how rapidly the octane levels will resume the rising trend, as more metallic lead slowly becomes available for making greater quantities of ethyl lead compound. As octane quality rises over present levels the disadvantage of the refiner without catalytic cracking equipment will increase. Gasoline made by catalytic cracking, without addition of ethyl lead, approximates 77 octane by the official ASTM Motor Method test, compared with 66 for gasoline generally similar in volatility made by the older thermal cracking operation. Catalytic gasoline shows an even greater improvement in the Research octane number, the comparison being roughly 86 Research versus 71 Research octane for the thermal cracked product. This higher differential in Research octane is credited by many, although not universally so, as contributing to better road performance, and consequently resulting in a more desirable product marketwise. In some parts of the country a premium of roughly one fourth cent per gallon is now being paid for gasoline with higher Research octane made possible by including catalytic cracked product in the final blends. If such price differentials in favor of catalytic gaso-

Jan 1, 1947

By William Loblowitz

A simplified system of flotation testing has been developed recently at the Bureau of Mineral Research of Rutgers University. The technique involves the known principle of skin flotation and can be used with minute quantities of sample and reagents in a beaker. A vessel containing the conditioned sample with added water and flotation reagents is held inclined and rotated slowly. Water-repellent particles come in contact with air and float on the surface of the liquid, while wettable particles are submerged. The float is poured off and filtered whereas the nonfloat remains in the beaker. The filtrate may be returned to repeat the process. This procedure can be made quantitative. Separations are obtained and are remarkably complete and repeatable. The effect of different reagents, optimum quantities, pH and other variables can be determined in a fraction of the time required for conventional testing. However, the method gives no information on the effect of frothers and the quality of froth to be expected in a cell, and it is not practical for particles finer than 200-mesh. Unlike other preliminary tests, separate float and nonfloat products are obtained, and their contents can be determined quantitatively by chemical analysis or grain counts. After the optimum reagent combination has been determined, the effect of fines and frothing may be verified in the conventional flotation cell. On the other hand, agglomeration-tabling can be directly duplicated from beaker tests. Procedure: Five to ten grams of sample are weighed into a 100-ml beaker. Flotation reagents and a small initial quantity of water are stirred together; additional water is then added to produce the proper water-solids ratio. The beaker is then tilted to 45" and rotated slowly. After three to five rotations, liquid and float are poured off and filtered; the filtrate may be recycled until the separation is completed. One test generally requires less than 10 min. Reagent concentration and pH remain quite constant because of the recycling of the filtrate. Two to four tests may be made simultaneously, and the effect of varied conditions may be observed by comparison. Considerable time is saved in preparation and handling since small quantities of sample suffice for a series of systematic tests. Repeatability One test was repeated four times under constant conditions. The sample used was a quartz sand containing approximately 24 pct feldspar and some clay aggregates. The +28-mesh grains had been screened out, and most of those finer than 100-mesh had been removed by hydraulic classification. The results are presented in Table I. For comparison, 500 g of the sample were separated by agglomeration-tabling using the same reagent combination and quantities as given in Table I. The weight percent float was 18.3 pct, composed almost entirely of feldspar and with only traces of quartz. Most of the remaining feldspar was recovered in a middling product with 2.2 pct by weight.

Jan 1, 1952

By C. F. Gates, H. J. Ramey

Recent literature shows that pronounced increases in oil recovery can result from the use of miscible systems in recovery operations. This literature also points out certain problems associated with maintaining miscibility, e.g., compositional changes resulting from alterations in pressure and temperature or from zone dilution. The purpose of the work described in this paper was to study miscible zones for possible use in waterflooding operations and examine the manner in which these zones break down. The fluid system selected for study was oil—terNary-butyl alcohol—water, which, because of its narrow range of miscibility, is ideally suited for investigation in short, linear systems. The laboratory-observed effects on oil recovery and zone stability of a number of variables are reported. Among the variables investigated were miscible zone size, viscosity ratio, length of travel, and interstitial water saturation. Results obtained with this system show that interstitial water adversely affects recoveries because of premature phase break. Salinity of the water further aggravates Ais situation. This effect, although pronounced for this system, would probably occur in any fluid system containing an alcohol. As expected, viscosity ratio has a decided influence on recovery efficiency and zone stability. The results also show that use of a suficieno zone size, even though the system has poor phase characteristics, yields higher oil recoveries than are obtained from straight water floods. Length-of-travel studies showed a square root relationship between zone growth and path length for favorable viscosity ratios. No such clear-cut dependence was observed under unfavorable viscosity conditions. INTRODUCTION As new oil reserves have become increasingly more difficult and expensive to find and develop, the oil industry has devoted more and more time and money to finding more efficient methods for exploiting known reserves. The increasing number of water floods is one manifestation of this attempt to improve oil recoveries from existing fields. Since considerable quantities of oil are by-passed by the waterflood process, it is only a partial answer to the problem. The search continues. Of late, several proposed processes have received the critical attention of investigators. Among them are gas drives, in situ thermal reactions and miscible displacements. The present paper is concerned with miscible displacements in conjunction with water floods. Recent literature1- reports that, under proper conditions, oil recoveries from LPG floods, propane sweeps, condensing gas drives, etc., approach 100 per cent of the oil in place in the region contacted by the flood. This literature also points out some of the problems associated with these processes, one of the main ones being the maintaining of miscibility. Compositional changes resulting from pressure and temperature variations or from zone dilution give rise to phase breaks and loss of miscibility, the conclusion being that, after loss of miscibility, much of the beneficial influence of the zone is lost.&apos; The results of the subject work show that, if sufficient zone material exists ahead of a phase interface, considerable improvement in oil recovery can be obtained. In order to increase our understanding of the behavior of miscible systems as they degenerate into immiscible processes, a laboratory system having rapid deterioration characteristics was needed. The fluid system oil—ter tiary-butyl alcohol (TBA)—water possesses these properties and was the system investigated. Although these fluids are different from those generally employed in miscible studies, an understanding of their behavior can be applied to other miscible slug processes. However, under conditions where mass transfer maintains a miscible system through multiple contacts, e.g., enriched gas drive or high pressure gas drive, the observed behavior of alcohol zones would not be applicable. The variables of interest were zone size, viscosity ratio, length of travel, initial water saturation, rate and core characteristics. Of these, only the effects of the following on zone breakdown and oil recovery are reported in detail: (1) zone size, (2) path length, and (3) initial water saturation. The effects of viscosity ratio and core characteristics are discussed in conjunction with other variables. Although initial water saturation is not envisioned as important to the phase behavior of hydrocarbon systems, e.g., LPG, it is important in alcohol systems. The properties of the fluids and cores used are given in Table 1. As previously stated, this fluid system was selected because of the limited range of miscibility

By L. E. Tanner

A study was made of the transformation kinetics of the commercial titanium-base alloys, Ti-2.5Al-16V and Ti-4A1-3Mo-1V, using two different heat treatment cycles: 1) step-quenching to aging temperatures from a ß solution anneal and 2) water-quenching from an a+ß solution anneal followed by reheating to aging temperatures. Metallographic examination and hardness testing provided the major portion of the data, while electrical resistivity, dynamic elastic modulus, and X-ray diffraction techniques were also used to obtain critical or confirnzatory data. TTT diagrams were constructed from these results. The sheet alloys, Ti-2.5Al-16V and Ti-4Al-3Mo-lV, are of current interest to the Department of Defense. As an aid to the planning of their respective heat treatments, a program was carried out to determine the transformation kinetics of these alloys using ß and a + ß reference states. This paper presents the TTT diagrams constructed from data obtained by metallographic examination and hardness testing, as well as by X-ray diffraction, electrical resistivity, and dynamic elastic modulus determinations. EXPERIMENTAL PROCEDURE Materials—Sheets of the alloys were obtained from the producers in the "mill anneal&apos;&apos; condition and were tested prior to shipment to assure their meeting mill specifications. Chemical analyses were also supplied and are presented in Table I. Heat Treatment—The majority of the data presented in this study were obtained from hardness testing and metallographic examination. Sample coupons were cut from the alloy sheets and heat treated on a mass scale. The annealing cycles were operated in the following manner: 1) The ß solution anneals were carried out in a horizontal tube furnace with the bare samples protected by a dynamic helium atmosphere. Following this treatment, the samples were quickly transferred to lead, solder, or oil-bath furnaces for aging. After prescribed times at the various reaction temperatures they were water-quenched. 2) The second cycle simulated commercial practice, which requires the alloys be quenched to room temperature following the a + ß sotution anneal. This anneal was carried out in a muffle furnace with a dynamic helium atmosphere. The specimens were then reheated from room temperature to the reaction temperatures in lead, solder, or oil-bath furnaces, followed by water-quenching after prescribed times at these temperatures. Information concerning the critical temperatures of the alloys was obtained from the literature and solution treatments were based on these values. A summary of the solution annealing treatments is found in Tables II and 111. The aging temperatures for the (a - ß alloys ranged in 50°C intervals from 200°C (392oF) to approximately 50°C below the ß/a + ß transus in the first cycle and approximately 50°C below the a + ß solution temperature in the second. The transformations in these alloys were known to be rather rapid, and thus aging times started at 0.5 min and went to a maximum of 7000 min. Hardness Testing and Metallographic Preparation— Heat-treated samples were sheared and mounted in Bakelite with their cut edges exposed. After a flat surface was ground, the hardness was determined in Vpn on an Armstrong-Vickers machine utilizing a 20-kg load. Three to four impressions were made on each specimen. After this procedure, the hardness impressions were removed and the edge surfaces of the specimens were prepared for metallographic examination in the usual manner. The etchant was 20 pct HF and 20 pct HNO3 in glycerine. Electrical Resistivity—It has been shown that the isothermal reactions in titanium-base alloys can be followed by measuring the changes in e1etrical resistivity attending these transformations. As mentioned earlier, the reaction kinetics of a-ß alloys are rather rapid; thus, it would be expected that resistivity data obtained from these alloys would be more significant if measurements were made continuously at the respective aging temperatures. To accomplish this end a special apparatus, based on the current-potential principle, was assembled. Its design was derived from earlier devices constructed by Colner and zmeska1 4 and Levinson.5 The set-up provided for the heat treatment zof machined specimens (approximately 2 x l0-4in. in cross section by 3 in. in length) and the determination of their relative

Jan 1, 1962

By Dale A. Vaughan, Oliver M. Stewart, Charles M. Schwartz

Solid-solubility limits at 1500°, l000q and 500°C for carbon, nitrogen, and oxygen in high-purity tantalum were determined by X-ray lattice-parameter methods. For carbon, the solubility was found to be 0.17 at. pct at 1500°C, and less than 0.07 at. pct at 1000°C. A nitrogen solubility of 3.70 at. pct at 1500° C decreases linearly with temperature to 2.75 at. pct at 1000°C, and 1.8 at. pct at 500°C. In the case of oxygen, the solubility was found to be 3.65 at. pct at 1500°C, 2.95 at. pct at 1000°C, and 2.5 at. pct at 500°C. The phases Ta2C, the low-temperature modification of Ta205, and Ta,N of unknown composition but which has a superlattice structure based upon the original bcc tantalum lattice have been identified as the initial precipitates in the respective systems. Metallographic methods were employed to verify the X-ray analyses. The etching behavior of Ta is discussed in terms of lattice i?rzperfections and precipitate phases. The excellent fabricability, high melting point, and nuclear properties of tantalum are responsible for interest in this refractory metal. Data on the solid solubility of the interstitial elements (oxygen, nitrogen, and carbon) in tantalum and on the precipitate phases are somewhat limited. The significant contributions are discussed below. Because the purity of electron-beam melted tantalum (only recently available) is considerably higher than that used in previous studies, the present investigation was initiated. Gebhardt et all-3 have investigated the tantalum-oxygen and tantalum-nitrogen systems with particular reference to the changes in physical properties and to the rates of reaction between these gases and the metal. The solubility of oxygen in tantalum was reported2 to be 3.7 at. pet at 1500°, 2.3 at. pet at 100O°C, and 1.4 at. pct at 750°C. Schonberg4 reported that several oxide phases (Ta40, Ta,O, TaO and Ta,05) exist while X-ray studies by Gebhardtl showed only two oxides, Ta,05 and an unidentified phase which was associated with a platelet-type precipitate. La-gergren and Magneli,&apos; however, questioned the existence of compounds other than the two allotropic modifications of Ta,05 for the tantalum-oxygen system. In the case of nitrogen, the solubility was estab- lished by Gebhardt3 to be of the order of 7 at. pct at 1800°c. The solubility was reported to decrease rapidly with temperature, and, although no limits were established, a precipitate phase was observed by Gebhardt except when the high-nitrogen specimens were cooled very rapidly from the reaction temperature of 1800c. He reported the initial precipitate phase to be a tetragonal distortion of the bcc tantalum lattice while Schonberg6 reported the phase lowest in nitrogen Jo be a cubic super-lattice with a cell size of 10.11 A. Two other nitride phases, Ta,N and TaN, were reported; these appear to be isomor-phous with the carbides of tantalum. The tantalum-carbon system was investigated by Ellinger7 and by Lesser and Braurer. Two compounds, Ta,C and TaC, were reported to exist, each with a range of composition. The solubility of carbon in tantalum was found to be practically nil at all temperatures. Thus, of the interstitial elements which are present in small amounts in high-purity tantalum, carbon might be expected to form precipitates. The present investigation was initiated to obtain additional data on the solid-solubility limits of these interstitials at 1500°, 1000°, and 500&apos; with particular emphasis on the distribution and the identification of the precipitate phases. EXPERIMENTAL WORK AND RESULTS In the present investigations of the solid solubility and of the precipitate phases in the systems tantalum-nitrogen, -oxygen, and -carbon, high-purity tantalum was reacted with high-purity gases, homogenized at 1800°c, and annealed at and quenched from 1500°, 1000,

Jan 1, 1962

By Milnor Roberts

CORNWALL, a Mecca for metal miners the world over, is easily reached from the southern coast of England. Passengers who land at Plymouth or Southampton can connect with a fast train from London called the "Riviera express," which traverses the beautiful counties bordering the English Channel. In Cornwall the traveler soon notices the pits and stock-piles of white china clay, and the metal mines, both placer and hard rock. The deposits are associated with granite batholiths, of which there are four principal ones, each a few miles in diameter. Tin mines are especially worked in the granite near its borders and also in the immediately surrounding Paleozoic slates. Copper and lead are no longer of importance here but tin is being produced steadily from several mines, with arsenic and tungsten as by-products. At the close of the war the man-power available. for these mines had been reduced to one-third of normal, and only now is it again reaching full strength. As mining in Cornwall antedates the Christian era, even a Nevada prospector would have to admit that "she&apos;s a permanent camp." SUB-TROPICAL CORNWALL Redruth and Camborne are industrial centers of the tin mining industry, but more tourist hotels are found in neighboring resorts such as St. Ives, a quaint fish-ing town on the Atlantic-side of the peninsula of Corn-wall, where the numerous cats descended from those mentioned in the ancient riddle-rhyme about St. Ives now occupy every doorstep and wall. Another charm-ing resort. Penzance on the shore of the English Channel, is known by name to the public through the opera "The Pirates of Penzance," but is of especial in-terest to students of nature for its palm trees and other subtropical plants, which thrive owing to the nearness of the gulf stream, although the latitude is that of northern Newfoundland, Winnipeg, and the northern end of Vancouver Island. Among the industrial plants at Camborne are those of Holman Brothers, Ltd., where drills and other forms of mining equipment are manufactured. At the Corn-wall School of Mines, which specializes on the district, the staff has assembled excellent collections of local ores, which repay study by a visitor.

Jan 1, 1928

By P. B. Liebermann

THE resistance to motion offered by mine cars is caused principally by: Rolling friction, flange friction, bending rails, bearing friction and wind resistance. With proper construction and with a fair amount of attention and care, that is, under favorable conditions, the first three items cannot be greatly improved. The wind resistance ordinarily is negligible on account of the slow speeds commonly used. The bearing friction, however, is a variable item, depending upon the design, the bearing material, the lubrication, the location (whether in wheel-hub or on car-body) and the alignment. Under the most favorable conditions the bearing friction will reach a lowest possible value. By the development of a successful anti-friction mine-car bearing this lowest value has been improved to such an extent as to affect the whole system of mine haulage. After being satisfied of their durability and certainty of operation, any investigation into the advantages of anti-friction bearings for mine cars will have to be based upon reliable information as to the saving in power of such bearings. While numerous tests have been made in this direction, the results have not always been convincing, principally because of the rather crude methods that were employed. These crude methods are the main cause of the wide variations existing in regard to the exact amount of the frictional resistance. Frequently an ordinary spring balance is used and the pull necessary to move a certain car or train of cars is obtained by a number of readings. Such spring balances necessarily have a coarse graduation and the continuous vibration and fluctuations to which they are subjected make them highly dependent upon the individual observer. Further, they must be frequently calibrated. Sometimes these tests were made without regard to acceleration, speed or even grade.

Jan 6, 1916

By S. R. Goodman, Hsun Hu

A study has hem made of the formation of annealing textures in an 18-8 austenitic stainless steel (Type 304L) from various deformation textures obtained by rolling at different temperatures. When the deformation texture is a mixture of the ferritic type and the brass type owing to the pres -ence of both martensitic ferrite and retained aus-tenite in the specimen, recrystallization takes place by the growth of the existing austenite phase. In a previous report,&apos; it was shown that the rolling texture of austenitic stainless steel (Type 304L) changed gradually from the brass type to the copper type with increasing temperature of deformation above 200°C. These changes are similar to those in high-purity silver2,3 and electrolytic copper;4 a brass-type texture is favored at low rolling temperatures, whereas a copper-type texture is favored During the course of rolling -texture transition from the brass type to the copper type, the subsequent recrystallization textures change accordingly. The orientation relationship between the annealing textures and the various rolling textures, being consistent with previous observations on various fcc metals, can be described as [Ill] rotations of approximately 25 to 40 deg. Carhide precipitation may influence the annealing textures. at high rolling temperatures. Furthermore, the annealing textures in high-purity silver5 and electrolytic copper4 were found to depend entirely on the prior deformation texture. From a copper-type rolling texture a strong cube texture will form upon recrystallization, whereas from a brass-type rolling texture the annealing texture will be quite different from the cube orientation. In an earlier comm~nication,6 the formation of a strong cube texture in 18-8 austenite stainless steels (Types 304 and 304L) was reported briefly by the authors. The present paper constitutes the results of a complete study of the annealing textures obtained from a

Jan 1, 1965

By R. W. Diamond

THREE mills are now operated by the Consolidated Mining & Smelting Co. of Canada, Ltd.: (1) The Sullivan Concentrator, Chapman Camp, B. C. (near Kimberley, B. C.), (2) the, St. Eugene Concentrator, Moyie, B. C., and (3) the. Tadanac (Customs) Concentrator,Trail, B. C. Differential flotation is the only concentration method employed in all three plants. Tables are used for pilot work only. Values in all ores treated are as minerals of some or all of the metals -lead, zinc, gold or silver. Occasional customs ores contain small amounts of copper. Sulfide iron content of ores treated varies from a FIG. 1.-THE SULLIVAN CONCENTRATOR, CHAPMAN CAMP, B. C. (NEAR KIMBERLEY, B. C.). low figure in some ores to 38 per cent. iron in Sullivan ore. Gangue minerals vary considerably. A few customs ores are somewhat oxidized and as a result present difficulties. Flotation equipment and control are similar in the three mills, and the flow sheets at the St. Eugene and Tadanac mills, while much simpler, are modeled after that of the Sullivan Concentrator. In this paper I will not detail treatment nor equipment in any of our plants but will describe special features in, or in connection with, all of them. I will then deal with flotation reagents, describing our use of each of them, particularly where differing from general practice. I will conclude with comments on special subjects related to differential-flotation.

Jan 1, 1927

Discussion of the paper of S. E. Bretherton, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 80, August, 1913, pp. 1481 to 1487. S. E., BRETHERTON, San Francisco, Cal.:-Since preparing my paper, our chemist, F. L. Wilson, has been experimenting with Leadville, Colo., oxidized zinc ore and Leadville zinc sulphides containing lead, operating upon 40-1b. lots at a time. His results on Leadville sulphides are as follows: The raw ore contained a trace of gold, 5.04 oz. of silver, 19.1 per cent of zinc, and 7.24 per cent of lead. After roasting the ore contained a trace of gold, 5.72 oz. of silver, 0.75 per cent of copper, 21.7 per cent of zinc, and 8.29 per cent of lead. The loss in weight by leaching was 38.8 per cent. The extraction was 42.8 per cent of the copper, 80.6 per cent of the zinc, 7.1 per cent of the lead, 0.64 per cent of the silver, and no gold. The little .silver that is extracted would be thrown down with the copper when precipitating it from the zinc and both thrown hack into the residue to be smelted. There would be no trouble in smelting the residue with nearly all the sulphur eliminated and containing less than 7 per cent. of zinc. On zinc carbonates containing silicates the results are not satisfactory. H. O. HOFMAN, Boston, Mass. (communication to the Secretary*) :¬The paper by Mr. Bretherton upon the application of ammonia and carbonic acid to the recovery of zinc as oxide from roasted sulphide ore is of interest to me, as the first installation of the Schnabel process for the extraction of zinc from a mixture of zinc oxide, lead oxide (with some cupric oxide), and pellets of enriched lead, produced in steaming liquated zinc-silver-lead crust of the Parkes process, was made at Lautenthal, Harz mountains, where I was chemist. In that capacity I carried out numerous experiments on the Schnabel process, was active in the erecting of the plant, and later had charge of it. After the Lautenthal plant had been in operation for some time a similar one was built at Hoboken-les-Anvers, but both have been abandoned, as the wet process could not compete with the distillation of the liquated zinc-silver-lead crust, now used universally in the Parkes process.

Jan 11, 1913

Further discussion of the paper of JAMES JOHNSTON, presented at the New York meeting, February,. 1914, and printed in Bulletin No. 85, January, 1914, pp. 107 to 133. See also Bulletin No. 91, July, 1914, pp. 1473 to 1496. THOMAS CROWE,* Victor, Colo.-The interest manifested of late in the treatment of low-grade ores, together with Mr. Clevenger&apos;s discussion of the Mill and Metallurgical Practice of the Nipissing Mining Co., prompts me to acid a few remarks relative to concentration in connection with cyanide treatment of low-grade ores. Mr. Clevenger in this discussion does not condemn concentration in this connection, but, nevertheless, the tone of his remarks would lead one to believe that his conclusions are like those of many others: that concentration is often turned to as a last resort in an attempt to improve or obtain an extraction upon an ore by the recovery and sale of the refractory portion of the ore. This, I will attempt to point out, is not always the case. Concentration in connection with cyanidation often performs an entirely different function, i.e., one of saving fine grinding. Economy being the keynote of successful treatment of low-grade ores, the problem often becomes more commercial than metallurgical, and, as there is generally a definite ratio existing between cost of operation, degree of comminution, and percentage of extraction, the grade of ore under treatment usually imposes a limit upon these factors. With many ores grinding is the most expensive single item in their treatment; therefore, the degree of comminution is very apt to be governed by the allowable cost of operation. With most ores the degree of comminution controls to a great extent the percentage of extraction. So in the treatment of low-grade ore it often becomes necessary to sacrifice extraction, through coarse grinding for the benefit of cost, in order that the greatest ultimate profit may be obtained, and it is under these conditions that it is, possible for concentration to play an important part in overcoming to some extent the effect of mesh. The precious metals occurring in an ore are usually closely associated with the metallic portion of the ore, and as this metallic portion is generally fairly well liberated from the gangue at comparatively coarse meshes, further grinding of the ore is necessary only in order that the metallic portion may be reduced sufficiently fine that the precious metal part of it may be dissolved by cyanide solutions in a reasonable length of time.

Jan 11, 1914