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By Mark E. Smith

To allow recovery of gold values from ore which cannot be economically processed by the mill, Pinson Mining Company has developed a run-of-mine heap leaching facility. In order to estimate production scale recovery rates, reagent consumption and percolation problems, a series of pilot scale tests were performed. These tests typically consisted of 3,630 metric tons (mt) (4,000 tons) leach ore at a grade of .94 to 1.56 grams Au per metric ton (g/mt) (.03 to .05 oz. Au/ton). Test heaps were loader stacked to approximately 4.3 meters (14 feet) high. Information from these pilot scale tests was employed in the design and construction of the production scale facility. Parameters such as spray rate, leach cycle, sprinkler placement, and barren solution chemistry were determined by the pilot tests.

Jan 1, 1984

By L. R. Duncan, O. M. Wicken

Magnesium, the eighth most abundant element in the earth's crust, is found widely distributed in a variety of minerals. Among the more commercially important ones are magnesite (MgCO,), brucite (Mg[OH],) , dolomite (CaMg[CO,],), and the salts magnesium sulfate and chloride often found in natural brines. Among other commercially important magnesium-containing minerals are olivine ([MgFe],- SiO,) , talc (H,Mg,[SiO,],) , and serpentine (H,Mg,Si,O,) . These are valuable because of desirable characteristics given them by the magnesium content and its placement in the particular crystal structure. These minerals are the raw materials for a host of products including magnesium metal and several grades of magnesia or magnesia- containing materials for refractories, fluxes, fillers, insulation, cements, decolorants, fertilizers, and chemicals. Considering only those minerals valued for their magnesia or magnesium content, over 85% of the material tonnages are processed to be used as refractories. Dolomite, which is used in enormous tonnages for its physical properties in construction, has an important use as a refractory raw material in its own right and, after calcination, as a precipitant for magnesium hydroxide, which is an intermediate for the production of magnesia or magnesium metal. Magnesia from the reaction of calcined dolomite (or limestone) with sea-water or magnesium-containing brines has supplanted much of the production of magnesia from mined magnesite, particularly in the United States. The best known of the minerals directly and widely exploited for magnesia content is magnesite, one of the calcite group of rhombo- hedral carbonates which includes calcite (Ca- CO,) , siderite (FeCO,) , and rhodocrosite (MnCO,) among others. The members of this group enter into a wide range of substitutional solid solutions when the positive ions have similar radii. The radii of magnesium and iron ions are within 6% of each other; hence, magnesite and siderite form a complete series of which breunnerite (ferroan magnesite) is a well-known end member. However, the radius of calcium ion is 36% larger than that of magnesium ion, and only limited substitution exists at each end of the MgC0,-Cam, series. Dolomite is not a member of the calcite group, but results when calcium and magnesium ions alternate in equal number in an ordered structure among carbonate ions. The result of these relationships is that calcite and dolomite, often found intermixed with magnesite, occur commonly as identifiable crystal entities which can often be separated to a varying degree from the magnesite by various beneficiation techniques. Magnesite, when pure, contains 47.8% MgO and 52.2% CO,. The pure mineral is sometimes, but rarely, found as transparent crystals resembling calcite, but, preponderantly, magnesite contains variable amounts of the carbonates, oxides, and silicates of iron, calcium, manganese, and aluminum. Magnesite may be either crystalline or "amorphous" (cryptocrystalline). The crystalline form has a hardness of 3.5 to 4.0. The color may range from white to black with shades of yellqw, blue, red, or gray. The color is not a fundamentally significant indicator of purity, but in a given deposit, an experienced person can often roughly grade magnesite by assessing color and crystallinity. The crystalline form of magnesite occurs in

Jan 1, 1975

By A. E. Brugger

SOME 2,000 years ago Pliny is supposed to have said, "Out of Africa always something new." It may perhaps even now be news to a great many that the Belgian Congo has in recent years been producing approximately a quarter of a ton of diamonds annually. For that is what the 1 1/4 million carats, the recovery from 40-odd operating mines, and about 20 or 25 per cent of the world's normal consumption, amounts to. In 1915, first exploitation operations produced less than 50,000 carats from two mines. The rapid expansion of operations following the Euro¬pean war meant a most rapid development of a virgin land. The interior is now reached by air in one day from the mouth of the Congo River, where steamers unload mail and passengers from Antwerp. This trip formerly consumed 4 to 6 weeks by a narrow-gage, wood-burning, railroad around the rapids of the lower Congo and Livingston Falls; by river boat to the heads of navigation, Djoko Punda on the Kasai or Luebo on the Lulua; and thence by caravan of native porters over narrow-trails to head¬quarters on the Tshikapa. Hundreds of miles of automobile roads have been constructed over veldt and through forest, bridging streams and ferrying rivers. The railway from Capetown to the Katanga copper district to the East, once two months away by trail is now reached in 2 or 3 days over fair automobile highway. Native "boys" who a few short years ago wore little more than a smile and a string of beads and to whom a wheelbarrow was a complicated piece of machinery, are today driving Fords, tending boilers and engines and operating electrical equipment, or are capable mine workmen, machinists and artisans, and dressed in all manner of cast-off white man's clothing. Even as late as 1920, due to difficulties of securing and transporting machinery during and just after the war, the crudest hand operations were the rule for the excavation, sizing, and concentration of the diamondiferous gravel. All washing and concentration is now mechanized, using steam or electric power, and where operations are sufficiently large to permit competition with native labor costs, excavation and transportation are also accomplished by machinery.

Jan 1, 1932

By Louis D. Huntoon

CANADIAN gold production is forging ahead annually and the prospects are that it will continue to do so for many years. Table 1 shows recent annual increases. Production for 1933 will probably reach $70,000,000, and further increases are likely in 1934 and 1935. (Data for November and December, 1932, are estimated throughout this article.) The depression sent many prospectors to the woods so during the last two years many new gold areas have been discovered and are attracting real capital for exploration and development. Several mills came into production in 1932 and mills now under construction will start production in 1933. The offices of mining lawyers are busy. Capital for this new work is obtained from well financed mining companies, syndicates, and individuals who were fortunate enough to invest in the dividend-paying gold mines of the north country in the early days. Prospectors and capital are cooperating. An interest is always retained by the prospector or vender and usually a small amount of real money is given the prospector.

Jan 1, 1933

By E. T. Turkdogan, B. B. Rice

Desulfurization of limestone during and subsequent to calcination has been investigated using U.S. Steel's Rogers City quarry-Michigan limestone cut to 25-30-mm diam spheroidal shapes. The experimental observations indicated that the sulfur present as iron pyrite in commercial limestone is oxidized partly to SO, during calcination and partly converted to sulfides (FeS, CaS) and CaSO4. If calcination is carried out under oxidizing conditions, most of the sulfur is converted to CaSO4, which can be removed from burnt lime readily in CO,-CO mixtures, the higher the CO content the faster is the rate of reaction. In the 30-mm-diam spheroids gas diffusion in the pores of limestone and burnt lime is fast relative to rates of the desulfurizing reactions. Over the temperature range investigated, e.g., 850° to 1200°C, there is internal desulfurization.

Jan 1, 1974

By American Institute of Mining Engineers

David J. Mack (University of Wisconsin, Madison, Wise.)—Have the authors considered that the effects reported in their paper are readily explainable on the basis of equilibrium grain boundary segregation rather than ordering? It seems to the writer that all of their experiments and observations correlate well with known behavior associated with equilibrium grain boundary segregation. Although at first glance one would tend to dismiss such a possibility because of the similarity of the gold and copper atoms, their sizes differ by 12.8 pct which is in the range where segregation at grain boundaries would be expected. Then, too, the electrochemical differences between the copper, the Cu3Au, and the gold strongly suggest that a segregation mechanism is involved in the corrosion of the Cu-Au alloys. R. Bakish and W. D. Robertson (authors' reply)—The authors would like to thank Dr. Mack for his consideration of the problem of grain boundary segregation as an explanation of the observed phenomena. We had considered the problem in the following terms: Assuming a pure binary Cu-Au alloy and an ideal solid solution, the surface excess, T2= N25 — N2, of the second component (gold) may be expressed in the following way20 1 —exp (—da/kT) where 8 is the difference in surface tension of copper and gold, and a is the surface area per atom. In the present case, 6 is positive which implies that the component in excess at the boundary is gold. Since the only chemically active component in ferric chloride is copper, it does not appear that the segregation of gold is likely to increase the boundary activity. A small concentration of a third component could profoundly affect the situation. Analysis indicated only spectrographic traces of impurities, all of which are soluble in both copper and gold. Quenching experiments, reported in the paper, also tended to eliminate significant effects attributable to a third component.

Jan 1, 1958

G. SHERBURNE ROGERS,* Washington, D. C. (written discussion ?).- Mr. Neal's paper on the petroleum hydrology of the Mid-Continent district is a welcome contribution on a subject concerning which none too much is known; it is, I think, the first published description of the chemical character of the oil-field waters of the great Mid-Continent area. When studying the oil-field waters of the California fields several years ago, the differences in chemical composition between waters occurring at various horizons seemed to be sufficient to enable the operators to use water analyses as a basis for determining the source of the water flooding a well; and it is gratifying to find that, Mr. Neal has arrived at a similar conclusion. As Mr. Neal points out, the Mid-Continent waters are very different in character from those of the California fields, and casual. inspection

Jan 3, 1919

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who called at Institute headquarters during the period July 10, 1916 to August 1, 1916: W. A. Barnes, San Francisco, Cal. W. J. Mead, Madison, Wis. W. L. Bell, Davenport, Fla. Charles Mentzel, San Pedro, N. M. James P. Clarke, Jr., Little Rock, Ark. H. H. Miller, New York, N. Y. R. A. Carhart, Mitchell, S. D. W. E. Pomeroy, El Paso, Tex. G. M. Colvocoresses, Humboldt, Ariz. M. K. Rodgers, Los Angeles, Cal W. E. Defty, Phoenix, Ariz. S. C. Rodgers, Guanajuato, Mex. Carl F. Dietz, Worcester, Mass. John M. Baker and Hamilton W. Baker have resigned as general manager and mine superintendent respectively of the Baker Mines Co., of Oregon. After Aug. 1, their address will be 43 Emerson St., Denver, Colo.

Jan 9, 1916

All the TECHNICAL PUBLICATIONS and CONTRIBUTIONS published in 1936 arc available at Institute headquarters, unless otherwise noted They are also on file in many public, university and technical libraries and, when so indicated in the list, may be found in the TRANSACTION Copies of the TECHNICAL PUBLICATIONS have been mailed to members of the Institute that are registered in the different classes A-Metal Mining, B-Milling and Concentration, C-Iron and Steel Division, D-Nonferrous Metallurgy, E-Institute of Metals Division, F-Coal Division, G-Petroleum Division, H-Industrial Minerals Division (Nonmetalhcs) , I-Mining Geology, L-Geophysical Prospecting Other members may obtain copies by writing to the Secretary Copies of CONTRIBUTIONS may also be obtained from the Secretary's office Additional copies are sold at the rate of 1 cent per page, minimum charge, 25 cents Non-members may purchase the papers to the prices mentioned

Jan 1, 1937

By Donald L. Katz, Marshall B. Standing

Density data are reported on 16 saturated hydrocarbon vapors at Pressures ranging from 1000 to 8220 Ib. per sq. in. and at temperatures ranging from 35° to 250°F. These data have been used to extend the compressibility-factor chart for natural gases up to 10,000 lb. per sq. in. The relatively large quantity of high-boiling constituents present in high-pressure vapors in equilibrium with crude oils makes it necessary to include in the analysis of the gas the molecular weight, density, and possibly boiling range of the heptanes and heavier fraction. Relationships have been presented by which the density of gases may be obtained directly from the temperature, pressure, and gas gravity provided the gases have a common source or are similar in composition. Introduction The densities of natural gases are necessary in many engineering in in petroleum production and utilization, Gas reserves, changes in reservoir pressure, gradients in gas wells, metering of gases, pipeline flow, and compression of gases are typical problems requiring the density of the gas. A decade ago, engineering computations used ideal gas laws with deviations up to 500 Ib. per sq. in.4 Recent discoveries of pools having Pressures UP to 7500 lb. Per sq. in., and installation of pressure-maintenance and recycling plants, have increased the need for data On gas density at high pressures. Methods of Computation The accepted method of computing the density or specific volume of natural gases is the use of the ideal gas law corrected by a compressibility factor. The method proposed by Kay7 of correlating compressibility factors for gaseous mixtures on pseudocritical properties5 appears to be satisfactory for natural gases.2 The meth-me-compressibility factor has been shown to deviate systematically from the behavior of natural gases2 and a chart giving these corrected factors is available. A method of computing specific volume of gaseous mixtures from partial molal volumes has been reported by sage and Lacey.8 Complete data for the computation are not yet available for all hydrocarbon gases. Most- of the reported data on gas densities have been in the single-phase region removed from the dew point or saturation condition. Since most gases in the reservoir Or while on contact with liquid '''ring flow are saturated, the determination of densities under conditions of saturation is particularly important. Although there is no reason to believe that the saturated gases differ in behavior from those consider. ably removed from their dew points, the usual experimental determinations find difficulty on approaching the dew-point conditions, This paper reports the density of I6 saturated gases in equilibrium with crude oils. The relationships developed to compute the density of gases to high pressure' have been modified and enlarged. A simpli-fied method of obtaining gas density is presented in the Form of charts, which apply for specific groups of gases.

Jan 1, 1942

By Marshall B. Standing, Donald L. Katz

Density data are reported on 16 saturated hydrocarbon vapors at Pressures ranging from 1000 to 8220 Ib. per sq. in. and at temperatures ranging from 35° to 250°F. These data have been used to extend the compressibility-factor chart for natural gases up to 10,000 lb. per sq. in. The relatively large quantity of high-boiling constituents present in high-pressure vapors in equilibrium with crude oils makes it necessary to include in the analysis of the gas the molecular weight, density, and possibly boiling range of the heptanes and heavier fraction. Relationships have been presented by which the density of gases may be obtained directly from the temperature, pressure, and gas gravity provided the gases have a common source or are similar in composition. Introduction The densities of natural gases are necessary in many engineering in in petroleum production and utilization, Gas reserves, changes in reservoir pressure, gradients in gas wells, metering of gases, pipeline flow, and compression of gases are typical problems requiring the density of the gas. A decade ago, engineering computations used ideal gas laws with deviations up to 500 Ib. per sq. in.4 Recent discoveries of pools having Pressures UP to 7500 lb. Per sq. in., and installation of pressure-maintenance and recycling plants, have increased the need for data On gas density at high pressures. Methods of Computation The accepted method of computing the density or specific volume of natural gases is the use of the ideal gas law corrected by a compressibility factor. The method proposed by Kay7 of correlating compressibility factors for gaseous mixtures on pseudocritical properties5 appears to be satisfactory for natural gases.2 The meth-me-compressibility factor has been shown to deviate systematically from the behavior of natural gases2 and a chart giving these corrected factors is available. A method of computing specific volume of gaseous mixtures from partial molal volumes has been reported by sage and Lacey.8 Complete data for the computation are not yet available for all hydrocarbon gases. Most- of the reported data on gas densities have been in the single-phase region removed from the dew point or saturation condition. Since most gases in the reservoir Or while on contact with liquid '''ring flow are saturated, the determination of densities under conditions of saturation is particularly important. Although there is no reason to believe that the saturated gases differ in behavior from those consider. ably removed from their dew points, the usual experimental determinations find difficulty on approaching the dew-point conditions, This paper reports the density of I6 saturated gases in equilibrium with crude oils. The relationships developed to compute the density of gases to high pressure' have been modified and enlarged. A simpli-fied method of obtaining gas density is presented in the Form of charts, which apply for specific groups of gases.

Jan 1, 1942

By G. P. Conard, E. H. Rennhack

The generation of fibers composed of individual TiZn15 compound particles and their influence on crystallographic orientation in chill-cast, hot-rolled hypoentectic Zn-Ti alloys were explored. Metallo-graphic examination and X-ray diffraction data show that such fibers form a planar network after 50 pet reduction which eventually tends to suppress twinning at some critical reduction level (-90 pct) where the grain size approaches the interfiber, spacing. This leads to the development of a duplex-type projerred orientation through slip rotation consisting of an al-most ideal (0001)(2iiOj texture and a (0001) (1010) rotated component. Correlations between basal-plane rotation and secondary- creep rc11e sugg-est, however that prejerred orientation does not contribute in a major way to the creep resistance of these alloys. EFFORTS to improve the creep resistance of zinc through alloying without incurring a loss in fabricating properties have achieved only minor success with the exception of the very effective addition of titanium. Anderson, Boyle, and Ramsey,l for example, demonstrated that increasing the amount of thiselement from 0.05 to 0.23 wt pct produced a progressive, 45-fold increase in the inverse creep rate of hot-rolled

Jan 1, 1967

By R. Bakish, M. A. Badiali, N. W. Kirshenbaum

One pound of ultra pul-e molybdenum has been produced containing both metallic and nonmetallic impuvities close to or less than the limits of detection. various purification methods were investigated; althouglz the use of move than one purification step was consideved, it was found that a single, caefully-controlled sublimation of MoCl5 yielded a highly puvified product without prior treatment or recourse to repeated sublimation. Hydrogen reduction of MoC1, to metal was attempted at atmospheric pressure; however, reduced pressure was necessary to obtain substantial yields. The tubular deposits of metal were consolidated into bulk fovm by electron beam melting undev high vacuum yielding a very low gas content. Boblems involved in monitoring the puvity of these materials and analytical results obtained are also presented. THE pronounced effect of even trace amounts of impurities upon fundamental properties of materials is well known to metallurgists and solid-state physicists. Consequently, groups interested in basic studies of metals have in recent years immensely stimulated the preparation and production of numerous ultra-pure metals. Increased demand by scientists for these high purity materials has necessitated development of facilities to prepare them in significant quantities; the procedures reported here were devised to produce significant quantities of ultra-pure molybdenum. Previous work performed in the field of vapor phase purification and hydrogen reduction of several other refractory metal chlorides had demonstrated valuable techniques applicable to molybdenum.' Various purification and reduction steps were individually investigated. Those procedures which showed the most favorable results with respect both to attainment of high purity and to ease of operation were then incorporated in the process utilized to produce the metal.' STARTING MATERIALS It is well known that because of differences in volatility, chlorides may be separated by fractional distillation. It was presumed that distillation of molybdenum pentachloride offered a simple and straightforward method of purification due to its relatively low boiling point. Alternatively, sublimation of the solid chloride also appeared feasible since MoC15 has both a reasonably narrow temperature range in which it exists as a liquid (a property typical of refractory metal chlorides) and a low enthalpy of sublimation. Pertinent thermochemical data of MoC15 are given in Table I. It should be noted that this compound must be handled with care as it is extremely hygroscopic. Anhydrous MoC15 was obtained from the A Metal Climax Co. METHODS OF PURIFYING MOLYBDENUM PENTACHLORIDE Distillation. It was expected that distillation methods, while affording an efficient purification, would prove simple to control and would have a higher production rate than sublimation processes. Also considered was the possibility of effecting a high degree of purification by using both these volatilization methods in conjunction—possibly a distillation followed by sublimation of the solidified condensate. Distillation of MoC15 was investigated using a single stage distillation column packed with chemically resistant glass beads. Heating coils were wound around the column and collection tube (condenser). As-received MoCl5 was charged into a flask connected with the column using a side loading arm under an argon flow. After the column and condenser were brought to about 270" and 210°C, respectively, the apparatus was lowered until the flask was fully immersed in a constant temperature fused salt bath maintained at about 285 °C. Distillation was continued for about 10 or 15 min until 50 to 70 g of distillate had been collected. Analyses of these distillations indicated that several elements, e.g., Cu, Fe, Ni, Cr, and Mg, were lowered in quantity although not all were removed to the same extent. The occurrence of Na, B, Si, and A1 in the distillates appeared to be due to contamination, possibly from corrosion of the pyrex glass. An improved distillation system of larger capacity and longer distilling column was built. Improvements were effected in lowering the amounts of such impurities as B, Mn, Ni, Na, Mg, Cr, Cu, and Fe. These studies were pursued concomitantly with efforts to purify by sublimation; it was subsequently found that although improvements in purity were obtained by distillation, sublimation processes were simpler to control and effected a high degree of purity.

Jan 1, 1963

By NORMAN EBBLEY

NUMEROUS references have been made recently to "Alaska's oil reserves," and in view of the wartime petroleum situation sober thinking demands a dispassionate and scientific study and investigation of these reserves or supposed reserves. The question naturally arises, "Is there actually oil in Alaska, or are the reserves there a supposition?" True, in 1923 President Harding established Naval Petroleum Reserve No. 4 in Alaska, certainly implying that oil was there. This reserve, embracing about 35,000 sq. mi., was set aside on the advice of the Bureau of Engineering of the Navy Department and was based upon the existence of known petroleum seepages at Cape Simpson on the Arctic coast. The Cape Simpson seepages have been known for more than fifty years, but in spite of persistent rumors of other seepages in northern Alaska no definite evidence of their existence has been available.

Jan 1, 1944

By L. J. Klinkenberg

It is pointed out that the current concept of pore size distribution is not unequivocally defined and that different methods aiming at a determination of such a distribution therefore do not lead to the same results. A pore size distribution should not be based on the idea that a core should, under all circumstances, behave as a bundle of straight non-interconnected capillaries of the same pore size distribution. This is illustrated by calculations and experiments on the displacement of miscible liquids. INTRODUCTION The introduction of the concept of pore size distribution has been an attempt to characterize the intricate geometry of the flow channels in porous media. As pores in a porous medium are interconnected it is impossible to describe exactly what is meant by a "pore" and, therefore, the term pore size distribution requires further amplification. In the visual method for the determination of pore size distribution "the pore" is considered to be the hole between the grains as observed on thin sections or on a polished surface of the rock under a microscope. In all other presently known methods,1,2 a displacement process is studied and it is ascertained what as- semblaae of straight cylindrical capillaries would show the same behavior. The distribution of the capillary diameters of this assemblage is said to represent the size distribution of the pores of the actual porous medium. From the foregoing it is already apparent that it is useless to try to decide which process or which method of investigation leads to a "correct" pore size distribution. To illustrate this further a displacement process in which a fluid is displaced by another miscible with it will be discussed and the results will be interpreted in terms of a pore size distribution. DISPLACEMENT EXPERIMENTS WITH MISCIBLE LIQUIDS OF NEARLY IDENTICAL VISCOSITY AND DENSITY Interpretation in the Form of a Pore Size Distribution If distilled water is displaced from a homogeneous unconsolidated sand pack by, for instance, a dilute solution of NaCI, the breakthrough recovery i.e., the amount of distilled water produced at the moment the first trace of NaCl can be detected in the effluent water, is between 95 and 100 per cent of the pore volume of the pack. This result can be understood by following in imagination the course of one particle of the liquid. Imagine a length, ?l, at the end of which a liquid particle has an independent chance of a renewed choice of pores of different diameters. In other words, the particle has a choice of traveling time, at, for any length ?l; instead

Jan 1, 1958

By T. B. Massalski, Horace Pops

The occurrence and the temperature dependence of the athermal martensitic transformation in bcc Cu-Zn ß-phase alloys have been studied by cold-state microscopy, differential thermal analysis, and electrical -resistivity measurements. CinenzatograpJzic studies have shown that in the majority of alloys the transformation occurs in two stages. A thermoelastic phase, having a 'needlelike" uppearance, forms initially at the MS temperature and grows relatively slowly, chiefly in the edge (lengthwise) direction. With further cooling, an additional martensitic phase forms in rapid bursts at a lower temperature, MB, Both martensitic phases appear to have the same cry stallographic habit hut their modes of formation and growth are different. For the composition range studied, between 38.55 and 41.49 wt pct Zn, the habit planes determined are close to the (2.17 ,12) plane of the matrix, in general agreement with the prediction of the phenomenological theory of martensite formation. Thermal cycling through the MB temperature produces permanent plastic deformation in the 0 matrix and gradutally eliminates the typical burst phenomena. Thermal cycling only through the MS temperature produces no noticeable deformation effects. THE bcc Cu-Zn ß-phase alloys tend to become unstable at low temperatures and undergo a martensitic transformation,'-3 but the details of the transformation have not been completely determined. Following earlier metal log raphic and X-ray work1 Tichener and ever' determined by means of electrical-resistivity measurements the temperature range of the martensite transformation during continuous cooling. The transformation temperature was found to decrease with increasing zinc content, becoming about -130°C for an alloy containing 40.04 wt pct Zn. Hull and Garwood3 made a metallo-graphic study of Cu-Zn 0 brasses at temperatures down to -160°C, and determined the habit plane of the transformation product for an alloy containing 38.88 wt pct Zn. No metallographic studies below liquid-nitrogen temperatures have been reported. The martensitic transformation in ß-brass alloys can also be induced by deformation.1,4 The MD temperature corresponding to the appearance of the strain-induced martensite is some 300°C higher than that observed without strain, and hence the transformation can be strain-induced in alloys containing a higher percentage of zinc. Massalski and Barrett4 found that alloys containing as much as 51.89 wt pct Zn could be transformed into a faulted hcp structure by cold working at liquid-helium temperature. Because the details of the MS temperature and morphology reported in the literature are somewhat incomplete, a further study has been made of some of the above features. A design of a cryogenic stage for optical metallography5 has permitted the examination of specimens at temperatures down to 4.2oK, and the use of a cinecamera has permitted a study of the morphology on cooling and heating. The particular aim of the present work was to examine the transformation temperatures, the habit planes, and the growth morphology over a wide composition range in the ß-phase field. The effect of thermal cycling upon the subsequent transformation was also examined.

Jan 1, 1964

By J. Leja, N. Sheikh

The stability of lead ethyl xanthate precipitate in aqueous environment of different pH (4.5 to 10.5) and at temperatures 25°C-60°C was investigated. Dissolution leads to a wide variation of pH, xanthate, and lead ions concentration in solution and to a deposition of solid products of reactions. X-ray diffraction patterns of these solids enabled identification of Pb(OH)3, PbCO3, and PbS as constituents of the remaining undecomposed Pb(EtX)1, together with some unidentified compounds (which give rise to intensive peaks with d values of 2.82A and 1.71A, and numerous peaks of lesser intensity).

Jan 1, 1974

By A. E. Wraith, N. J. Petch, J. D. Embury, E. S. Wright

The two most important parameters controlling the fracture behavior of a solid are its intrinsic properties, e.g.,grain size, and the operative stress system. The latter may be modified in laminates by the presence of weak interfaces. This is studied in notch-impact tests on a mode1 system of mild steel laminates containing a variety of interfaces. The effect of these is evaluated in terms of the ductile/cleavage transition. Two laminate geometries are distinguished, here called "crack-arrester " and "crack-divider". In both, cleavage is inhibited. This arises because of relaxation of a state of triaxial tension. In the crack-avrester laminates, cleavage initiated at a notch is confined to the layer containing the notch. In crack-cliuider laminates, a thick specimen behaves as the Sum of a number of thinner ones. Additional benefit may derive from improved intritnsic propevties of- the lanlinate layers arising from greater deformation in their manufacture. It has long been recognized that the two most important parameters controlling the fracture behavior of solids are their intrinsic properties (e.g., grain size friction stress,3 distribution of second phase particles4) and the operative stress system under which fracture occurs. In solids that show a ductile/cleavage transition, cleavage is favored by the presence of a notch. This is because triaxial tensions, generated by the localized plastic constraint at the notch, are operative when fracture occurs.= Anything that suppresses these triaxial tensions will be unfavorable to cleavage. Such suppression may possibly occur in laminates containing weak interfaces and the purpose of the present paper is to explore this possibility. Two basic laminate geometries, here termed "crack-avrester" and "cvack-divider", are examined. They are illustrated in Fig. 1. With the crack-arrester laminates, there is the possibility that, when the fracture crack approaches the interface, this, if weak, may delaminate due to the tensile stress acting parallel to the plane of the crack.= If this happens, energy will be used in delamination, the crack will be completely blunted, and the triaxial tension associated with the crack will be relaxed. To fracture the second portion of the laminate, crack reinitiation will be necessary and, because of the relaxation of the triaxial tension, this reinitiation will occur under conditions of nearly uniaxial tension, which are unfavorable to cleavage. Thus there is the possibility of cleavage suppression in the second and subsequent subunits of a crack-arrester laminate. With the crack-divider geometry, there is again the possibility of delamination at the interfaces. This will divide the crack into a series of cracks propagating through the individual laminate subunits. If these are sufficiently thin, the triaxial tension will be relaxed towards a state of biaxial tension in each of them. Thus, with the crack-divider laminates, there is again the possibility of cleavage inhibition. In the present work, these possibilities are explored using a notched impact test on mild steel laminates bonded with soft solder, silver solder or copper. Even if delamination does not occur, it is still possible that cleavage may be inhibited in laminates. With the crack-arrester geometry, the cleavage crack in the first layer may be blunted and arrested by plastic deformation in the laminate bond, if this is ductile. Partial relaxation of the stress transmitted ahead of the crack into the second layer will then result and this will reduce the significance of this stress in the fracture of the second layer. With the crack-divider geometry, there cannot be much effect in the absence of delamination unless a large amount of energy is absorbed in rupturing the ductile material. EXPERIMENTAL DETAILS The composition of the mild steel (wt pet) was: 0.04 C, 0.29 Mn, 0.01 Si, 0.006 P, 0.008 S. "As-received" plate was annealed for 2 hr at 900°C and slowly cooled to give a grain size of 0.04 mm. The laminates were made by brazing or soldering together mild steel plates 8 by 3 in. by various thicknesses. These were obtained from the annealed plate by machining, so that the intrinsic material properties were .kept constant. Laminates containing two to six steel layers were studied using standard Charpy V-notch specimens cut from the bonded plates. Standard homogeneous specimens from the annealed plate and subsize ones from the laminate components

Jan 1, 1968

By C. J. McHargue, J. C. Ogle

Lightly deformed columbiun single crystals which contained only parallel hoins or purullel and intersecting trains were annealed at 1000' and 1600"C. No re-crystallizntion occurred in specimens hawing only parallel twins. Only noncoherent twin boundaries nzipated at 1000°C but both coherent and noncoherent ones moved al 1600°C. Recrystallization occurred within a few minutes at twin intersections at 1000°C. The orientation 01 the recrystallized grains differed front that of both the matrix and deformation twins, but could he derired by (110) and/or(112) rotations. ALTHOUGH twinning in metals has been extensively studied, there have been no definitive studies of the annealing behavior of crystals containing deformation twins. Some effects observed after annealing deformation twins have been summarized by Cahn1 and Hall2. Any or all of these phenomena are observed: 1) The twins may contract so that the sharp edges of the lens become blunted, and eventually the twin may disappear entirely. 2) The twins may balloon out at an edge, giving rise to a large grain having the same orientation as the twin. 3) The specimen may recrystallize; i.e., new grains are nucleated and grow at the expense of the twins and the crystal immediately adjoining the twin. Such grains have orientations which are not present before. Contraction has been observed in iron,3 titanium,3, 4 beryllium,5 zinc,8, 7 Fe-A1 alloy,' and uranium.9 Long anneals at high temperatures are required to have any appreciable effect in these metals and only thin twins are absorbed. Lens-shaped twins are absorbed from the edges: the thin, almost parallel-sided twins are usually punctured in several places and each piece contracts independently. Absorption is very gradual and no sudden cooperative jumps have been observed. The expansion of a twin into a larger grain of identical orientation is unusual, but such growth has been observed in iron,"'" zinc,6 and uranium." Crystals which have been deformed simultaneously by slip and twinning recrystallize first in the area adjacent to the twin. New grains appear faster where the twins intersect: but isolated twins, especially if thick, can also give rise to new grains. This type of recrystallization occurs in zinc.6, 7, 12, 13 and beryllium.14 Reed-Hill noted, in a single crystal of magnesium, the nucleation of a recrystallized grain at a twin intersection which had the same orientation as the second-order twin and which grew into the highly strained matrix.15 Short-time annealing has been reported to cause no change in the deformation twins in vanadium,16 columbium, 17, 18 tantalum,19 tungsten,'' and zinc.7 The purpose of this investigation was to note the effects of annealing on the coherent and noncoherent boundaries of deformation twins in columbium and to locate the nucleating sites for recrystallization. The orientation relationships, which the new recrystallized grains have with the parent crystal and the deformation twins, were also determined. EXPERIMENTAL PROCEDURE Single crystals of columbium were obtained by cutting large grains from electron-beam-melted buttons which contained 10 to 50 ppm C, 10 to 100 ppm O,, 1 to 10 ppm H2, and 10 to 15 ppm N2. The crystals were hand-ground and chemically polished until all grain boundaries were removed. The specimens were mounted in an epoxy resin and a face of each crystal was mechanically polished on a Syntron polisher using Linde A and then Linde B polishing compounds. After all faces were mechanically polished, the crystal was electrolytically polished to remove all distortion due to cutting and grinding. Laue photographs were taken of all faces of the crystals to determine the quality and orientation of each crystal. The crystals were compressed about 10 pct at -196 C in a specially constructed compression cage with an Instron tensile machine. Each crystal was separated from the top and bottom anvils by teflon films which acted as a lubricant. With the specimen crystal in position, the entire cage was cooled to -196°C by being submerged in a Dewar containing liquid nitrogen. The crystals were compressed at a rate of 0.02 in. per min and the load was recorded on a strip-chart recorder. After deformation the crystals were mechanically polished on 600-grit paper and Pellon cloth with Linde A and Linde B polishing compounds. The crystal faces were chemically polished and then etched. The twin planes were identified metallographically from an analysis of the twin traces on two surfaces. Annealing was carried out by placing each crystal in a columbium bucket made from the same electron-beam-melted material as the crystal itself and suspending the bucket by a tantalum wire in a quartz tube. After a vacuum of 10-7 Torr was attained, a furnace at 1000" or 1600 C was raised into position and the crystals held for various lengths of time. The crystals were repolished and etched after annealing to remove any surface contamination. Approximately 0.010 in. was removed during this process. The resulting surface was examined metallographically for microstructural changes due to annealing. A microbeam Laue camera mounted on a Hilger Micro-focus X-ray unit was used to determine the Orientstions of the recrystallized grains. This X-ray micro-beam camera had a 0.002-in.-diam collimator and incorporated the ideas of both and and chisWik21 and Cahn.22

Jan 1, 1967

By C. S. Matthews, M. J. F. Rosenbaum

The purpose of thir work wax to lcarn it~lzut infori~lation could he obtained from various typs of pilot water floods and to attempt to find the optunum pilot patter11, for a revervoir which had previously been depleted by a solution gas drive. The study was made in the laboratory with mathemetical methods a dynamic analog and a potentiotnetric analog. Results werp tested against the field llistorics of a nrrnlber of pilot water floods. At a reasonable valrre of currzulative injection, the total production rate for the one-injector five-spot should reach about 6.5 per cent of injection rate, and for a four-injector five-spot, about 9 per cent. Accurate estimates of ultimate recovery cannot be made on the basis of such snzall prorluction rates. However, with a pilot composed of nine ir1jector.s and 16 producers the production rate is approximately 50 pcr cent of injection rate at a reasonable value of camulative injection. Sonle inforn~ation for extended performance predictions might he obtained from such a large pilot. These conclusions were drawn on the basis of results obtained for unit mobility ratio, and a sturly using tlre potentiometric analog was made of the effect of other mobility ratios to determine the range of applicability of these predictions. For the four-injector, five-spot pilot with the ratio of production to injection rate (before water breakthrough) is about twice that for with it is about two-thirds; and with M0= 10, it is about one-third For high mobility ratios, it was found that the production rate increased considerably as water-cut increased. These result can be used to modify, qualitatively, the inter.pretntions based on curves for the unit rnobilit\. ratio CaSeS. It was found that the maximum ratio of production rate to injection rate obseriled in field pilot floods was of rhe scime order as that prerdicted by these methods. The time required to reach thisr maximum did not generally agree with the time predicted for a homogeti~orir reservoir. The differcrlce between predicted and observed time of response gives an indication of the permeability profile and of the condition of the producin,g wells. Pilot water floods of the pattern type are generally carried out in reservoirs which have been depleted by solution gas drive and are at low pressure. Under these conditions, oil and water can be considered incompressible. It is assumed that, as the water is injected, an oil bank forms ahead of it and that there is a distinct interface between the water zone (or bank) and the oil zone (or bank) and between the oil zone and the region ahead of the oil zone. It is further assumed that only gas is mobile in the unflooded (gas) region, only oil is mobile in the oil bank and only water is mobile in the water bank. The saturations and the mobilities associated with each zone are assumed uniform. We idealize our reservoir to be homogeneous, horizontal and of constant thickness. Effects of gravity within the producing layer are assumed negligible. If the actual time-dcpendent flow problem is approximated by a acries of steady-state problems. the potential and stream function in the oil bank and water hank satisfy Laplace&apos;s equation in two dimensions. We can therefore use a poteiitiometric analog of this system. Potentiometric models have yielded uscful results in this laboratory&apos; and clsewhere in the study of a variety of secondary recovery problems. For the case where M = I, we generally prefer to use theoretical mcthods as well as a simpler dynamic analog. Except where otherwise noted, the ratio, side of five-spot/wellbore radius. is taken to be 3,600. a figure which corrcsponds to a normal-size wellbore in a 10-acre well spacing. THEORETICAL EVALUATION OF VARIOUS PILOT PATTERNS, Mw0 = 1 <&apos;he theoretical models which we used to examine the performance of various pilots are shown in Fig. 1. Image theory was used to determine the ratio of production rate to injection rate as a function of the volumc of the flood. The ratio of production rate to injection rate was chosen because this is an easily measurable quantity which is characteristic of a pilot