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By S. T. Wlodek

The surface and subscale oxidation reactions were followed by means of continuous weight-gain and metallographic techniques over the range 1600" to 2200°F (871° to 1204 °C) for up to 400 hr. Full identification of all scale and subscale reaction products was obtained by electron and X-ray diffraction. At or below 1800°F (982°C) a linear rate of reaction (QL = 46.0 kcal per mole) governed the oxidation process, extending for up to 100 hr at 1600°F (871 "C). During linear oxidation the surface scale consisted of an amorphous SiO2 film overgrown with Cr 2O 3 and NiCr204. This initial linear process was followed, and above 1800°F completely replaced, by two successive parabolic rate laws (Qp = 60 and 57 kcal per mole). This parabolic reaction involved the formation of a complex scale consisting of Cr2 O3 and smaller amounts of NiCr2O4. Parabolic oxidation appeared to coincide with the disruplion of the silica film present during linear oxidation and was followed by subscale (internal) oxidation of crystobalite and NiCr2O4. The balance between the subscale and surface oxidation reactions controls the oxidation of this commercial alloy. The amorphous silica film appears to result in the linear rate and diffusion through Cr2O3 is the more likely rate-limiting step during parabolic oxidation. THE oxidation of a multicomponent composition is a complex phenomenon not presently amenable to a rigorous classical interpretation. Nevertheless, even a qualitative understanding of the scaling and subscale reactions that occur in a commercial composition can illuminate the reactions that limit its high-temperature stability in an oxidizing environment. This study of the oxidation of Hastelloy Alloy X presents the first of a series of studies with the above approach in mind. Hastelloy X exhibits one of the best combinations of strength and oxidation resistance available in a wrought, solution-strengthened, nickel-base alloy. Although during long time exposure some precipitation of M6C and M23C8 carbides as well as a complex Laves phase occurs, the amounts are probably small enough to have no appreciable effect on the chemistry of the matrix. Radavich has identified the oxidation products on Hastelloy X oxidized for 5 min to 10 hr at 1115°F as NiO and the NiCr2O4 spinel. Oxidation for 5 to 15 min at 1500°F produced a scale of spinel, NiO, and a rhombohedra1 phase, probably Cr2Os. Sannier et 2. have reported continuous weight-gain data for Hastelloy X at 1650" and 2010°F and internal-oxidation measurements after 150 hr at 2010°F. In addition, much of the data on binary Ni-Cr alloys recently reviewed by Kubaschewski and okins' and Ignatov and Shamgunova4 as well as studies of binary Ni-Mo alloys5 are also pertinent to the oxidation of this composition. EXPERIMENTAL Continuous weight-gain measurements and metallographic measurements of subscale reactions were the main experimental techniques used in this study. X-ray and electron diffraction backed up by a limited amount of electron-microprobe analysis served to characterize the nature of the scale- and subscale-reaction products. Two heats of commercial sheet of the composition given in Table I and identified as A and B were used in the bulk of this study. Internal-oxidation measurements were made on a third heat of material in the form of a 0.5-in.-diam bar. In order to assure homogeneity, all heats were reannealed 4 hr at 2175°F prior to sample preparation. weight-Gain Measurement. All specimens (1.5 by 0.4 by 0.03 in.) were abraded through 600 paper, electropolished, and lightly etched in an alcohol-10 pct HCl solution. An electrolyte of 150 cu cm H,O, 500 cu cm HsPO4 (85 pct conc), and 3 g CrO3 at a current density of 0.9 amp per sq cm or a solution of 10 pct HaW4 in alcohol used at 4 v and 0.3 amp per sq cm was used for electropolishing. The resultant surface exhibited a finish of 3 ± 1 p rms. Continuous weight-gain tests were made at 1600°, 1700°, 1800°, 1900°, 2000", and 2200°F on auer' type balances capable of recording a total weight change of 110 mg with an accuracy of k0.1 mg. All tests were made in air dried to a dew point of -70°F and metered into the 2-in.-diam reaction

Jan 1, 1964

By Charles Janin

The first successful bucket-elevator dredge to operate in California was put in comnlisvion wt Oroville in March, 1898. There had been numerous previous attempts at dredging, but noue of the earlier boats proved a success. The gold-miners in California earl3 conceived the idea of a machine to dig gravel from the beds and bars of auriferous streams that were inaccessible by the methods then employed, and it was only a few months after the discovery of gold in California that such a machine was Shipped around Cape Horn from New York to San Francisco. Thij was, however, but the forerunner of many failures in gold-dredging, and was soon at the bottoni of the Sacramento river. During succeeding years many other unsuccessful attempts mere made, and it was not until 1897 that a dredge of the single-lift bucket-elevator type mas floated on the Yuba river. This dredge was built by the Risdon Iron Works for 12. H. Postlethwaite, and would probably have been a success if it had been operated on some of the rich Ororille ground

Jan 1, 1912

By K. E. Gray, G. M. Myers

In previous publications,5 results of single-blow bit tooth impacts on saturated rocks at various stress states were reported. This paper extends these earlier works to include study of bit impact tests on salt water-saturated Berea and Bandera sandstone samples under conditions of elevated confining and pore pressure. During the tests dynamic filtration and deposition of a mud cake were occurring due to the presence of drilling mud in the borehole and a borebole-to-formation pressure differential. Results indicate that saturation of these sandstones with salt water tends to make them weaker than when saturated with nonreactive fluids. Plastic failure often occurs even when extremely high fluid-loss muds are present in the borehole. The failure mode tends toward plasticity with decreasing fluid loss. Brittle failure of sandstones in mud-filled holes is apparently relatively rare. Depending on the stress level, and the associated failure mode, withdrawal of the bit tooth induces a tensile force that seems rather important relative to the quantity of rock removed by vertical tooth impact. INTRODUCTION A vast majority of the oil wells drilled today involve the use of colloidal muds having a measurable mud filtrate loss. It is known from field experience that reduction of the water loss of a mud generally results in a reduction of the penetration rate. This paper describes an investigation of crater formation at simulated bottom-hole pressure conditions for drilling fluids having different water losses. The literature on single bit tooth impact (cratering) at atmospheric conditions is extensive, but only a limited amount of work has been performed at the stress conditions similar to that found in oil wells. Spherical penetrator cratering tests on rocks at hydrostatic pressure were performed by Payne and Chippenda1e.1 Chisel impact studies on limestone with independently varying overburden and borehole pressure and atmospheric pore pressure were reported by Garner, et al.2 Gnirk and Cheatham3 performed "static" penetrator tests on dry rocks at equal overburden and borehole pressures. Podio and Gray4 studied the effect of pore fluid viscosity at atmospheric pore and borehole pressures and varying overburden pressures. Their results illustrated the importance of fluid saturation of the rock. Yang and Gray5 reported single tooth impact tests on saturated rocks at elevated borehole, pore and confining pressures, but with equal pore and borehole pressures. For the work reported in Refs. 4 and 5, filtration across the hole bottom purposely was avoided. Maurer6 has investigated the effect of independently varying pore and borehole pressures at elevated overburden pressures by using a zero water-loss mud in the borehole. His tests were carried out under conditions that allowed independent control of overburden, pore and borehole pressures, but without control of filtration at the hole bottom. EXPERIMENTAL APPARATUS AND PROCEDURE APPARATUS The single blow chisel impact apparatus used by Garner,2 as modified for this study, is shown in Fig. 1. A cross section of the pressure vessel is shown in Fig. 2. Several pieces of auxiliary equipment were added to the original apparatus in order that the borehole and pore pressure could be applied in a manner analogous to the actual bottom-hole situation. The pore-pressure system included a filtrate volume-measuring transducer and had sufficient surge capacity to allow filtrate to be injected into the sample without significant changes in pore pressure at points remote to the borehole. The borehole-pressure system contained a cross connection to the pore-pressure system so that both systems could be pressured simultaneously. The borehole-pore pressure differential was applied rapidly by the use of a quick and full-opening valve. The operation of this valve triggered two industrial

Jan 1, 1969

By L. R. Jackson

THE idea presented in this paper is that the capacity of a metal for plastic flow before rupture is dependent on the type of stress system applied-that is, the absolute magnitude of the stresses are unimportant provided that they are large enough to produce continued flow; the important factor is the "type" of stress system. A term called the "triaxial stress ratio" is defined in such a way that this ratio can be used to characterize the "type" of system. The paper is divided into three sections. The first section discusses means of representing the effect of complex stresses on plastic flow and defines "triaxial stress ratio"; the second section discusses various methods of' obtaining complex stress distribution. The third section gives some experimental results showing the effect of types of complex stress on the capacity of various metals for flow. An appendix discusses some details on methods of obtaining complex stresses. I. REPRESENTATION OF COMPLEX STRESS SYSTEMS AND THEIR EFFECT ON PLASTIC FLOW Representation of Stresses It is convenient to have a consistent system of notation that will allow the representation of the entire range of complex stresses from hydrostatic compression to hydrostatic tension on plastic flow in a single diagram. Such a system is provided by making use of the fact that any complex stress system can be resolved into a hydrostatic tension or compression and a pure shear. Consider a stress system having the principal stresses [S1 S2 5 S3]. This system can be resolved into a new system consisting of the three components [ ] and three pure shears. If Sm is positive, the net stress effect is hydrostatic tension; if it is negative, the effect is hydrostatic compression. In order to produce a systematic notation, a quantity that will be referred to as the "triaxial ratio" will be defined by the equation [ ] Sm is given by Eq. I and S1 is the absolute magnitude of the largest principal stress without regard to sign. Table I lists the triaxial ratios for various common systems. [ ] Representation of Strains Strains will be plotted as "true" strains according to the system proposed by Ludwik.1

Jan 1, 1944

By G. U. Greene

The various lead producers have given the subject of lead drosses much attention in recent years but the problem of their economical treatment is yet to be solved. Formerly the copper in the furnace feed was removed from the furnace in the form of matte. The speiss at that time consisted principally of the iron arsenide. The practice today is to roast off most of the sulphur and the copper in the feed forms a dross in the furnace, which is removed from the furnace with the lead. This material is poured into the drossing kettles and allowed to cool down to but slightly above the freezing point of lead. The copper dross, containing almost all of the arsenic and part of the antimony, is skimmed off and treated in a small reverberatory furnace at most plants. This is essentially a liquation process. The skimmed dross contains from 70 to 80 per cent lead, and much of this lead is liquated out. The products from this treatment are: (1) impure lead, (2) speiss and (3) matte. The speiss from the reverberatory furnace was studied in this research. The literature on the subject is of very little assistance, as almost no work has been done on the problem of establishing the exact identity of the various phases present. One author(1)† states that speiss consists of a series of isomorphous compounds of the general formula FexAsy in which the Fe may be replaced by Ni, Co, Cu, Pb, Ag, Au, Pt, Zn, Cd and the As replaced by Sb, S and Bi. Hofman(2) states that the iron arsenide present is Fe5As. Experimental Work In the present research, the author used for methods in an attempt to determine the composition of the various phases: (1) chemical, (2) microscopic, (3) roentgenographic and (4) thermal. Previous to this research, considerable time had been spent making analyses of different speisses, but unfortunately no very definite conclusions could be made as a result of these analyses.

Jan 1, 1937

By G. Bruggeman, K. G. Kreider

Grain boundary dij]usion coefficienls were measured in tungsten between 1400° and 2200° C and can be expressed by the equation sq cm per sec This activation energy confirms some eavlier estimates made .from tungsten sintering experiments. Grain boundary diffusion was found to occur in sub-bozrndavies having -misorientations of less than 10 deg. The actiuation energy for this subboundavy diffusion is equal to that for dijjusion in incoherent grain boundaries with in the limits of error. This is shown to be consistent with the dislocation model of Low-angle boundaries wheve diffusion occlcvs along- the dislocation 'YPipes" comprising -tile boundary. RECENT investigations of the sintering of tungsten powders all report activation energies which are considerably less than the activation energy for tungsten volume diffusion. Kothari' reports a value of 100 * 5 kcal per mole, Hayden and Brophy' obtained 90 kcal per mole, and Vasilos and smith3 found 110.7 kcal per mole from their sintering studies. Since most determinations of the activation energy for volume diffu-sion4-' fall between 120 and 160 kcal per mole (the true value seems most likely to be nearer 150 kcal per mole), the conclusion is drawn that the mass transport leading to densification during sintering is accomplished by grain boundary diffusion. This interpretation is consistent with various diffusion models of the sintering process. 10-12 Vasilos and Smith calculate diffusion coefficients from their data which fit the equation D * 1.36 x 10* exp(-llO,700/HD However, no direct measurements of tungsten grain boundary diffusion have been made. Furthermore, considerable disagreement exists between the directly measured values of tungsten volume diffusion.'-' In order to corroborate the inferred results of the sintering experiments concerning grain boundary diffusion and to provide accurate diffusion data essential to the analysis of the kinetics of creep, oxidation, precipitation, and so forth, the present work was undertaken to measure self-diffusion in single-crystal and polycrystalline tungsten between 1400" and 2200°C. It is within this temperature range that tungsten sintering is done, the re crystallization of tungsten occurs, and the widest application of tungsten as a high-temperature material will probably be made. EXPERIMENTAL PROCEDURE Radioactive WlE5 was produced by irradiating tungstic acid in a neutron flux of 1.2 x 1012 neutrons per sq cm per sec for 36 hr. A 2-week waiting period was allowed for the decay of w"~ also produced by the irradiation. (w"~ has a half-life of 24 hr.) The half-life of the remaining isotope was determined to be 75 days confirming the presence of w lE5 and the absence of any undesired radionuclide. Specimens 4 in. in diam and $ in. thick were cut from polycrystalline swaged tungsten rods (recrystal-lized) and from Linde single-crystal rods. Chemical analyses of these materials appear in Table I. Actually upon closer examination, the single-crystal specimens were found to consist of several subgrains separated primarily by tilt boundaries in which the misor-ientation ranged from 3 to 10 deg. Thus, it was possible to measure boundary diffusion coefficients in these low-angle subboundaries as well as in the incoherent boundaries of the polycrystalline specimens. The two faces of each specimen were ground flat and parallel within 0.0001 in. The radioactive tungstic acid was dissolved in concentrated ammonium hydroxide, placed on the ground flat of the specimen, and evaporated to dryness. The oxide was then reduced in hydrogen at 1000°C resulting in a layer of wlE5 approximately 1 p thick. The diffusion anneals were performed in vacuum in a tantalum resistance furnace. Time at temperature ranged from 10 hr at 1400°C to 2 hr at 2200°C. The penetration profile was determined by measuring the residual activity after successive removal of surface layers by grinding on metallographic polishing paper. Extreme care was exercised to insure that sections were always taken normal to the diffusion direction; this was verified repeatedly by checking that front and back surfaces of the specimen remained parallel. The activity was measured with an end-window Geiger-Mueller counter. The sides and edges of the specimen were well-shielded to eliminate possible effects due to surface diffusion. The weight of the

Jan 1, 1968

By George R. St. Pierre, John Chipman

METALLURGISTS have been studying the chem-ical behavior of sulfur in steelmaking for many years in order to have a better control of the sulfur content of finished steel. During the refining period in the open hearth, molten steel is separated from a gas phase by molten slag. Chemical reactions occur principally at the slag-metal interface and at the slag-gas interface. A need for physical-chemical investigations of reactions between sulfur-bearing gases and steelmaking slags was recognized some time ago.'.' From the early work, it can be qualitatively concluded that increased sulfur content and low partial pressure of oxygen in the gas phase favor the passage of sulfur from gas to slag. Using radioactive sulfur S Koch and Fink' have demonstrated the rapid rate of exchange of sulfur between gas and slag in an open hearth furnace. Gurry and Darken and Darken and Shields (as reported by Derge and Marshall') have equilibrated lime-iron oxide slags with SO—O2 gas mixtures. The major conclusion from the reported results is that sulfur content increases with increasing lime content in lime-iron oxide slags equilibrated with a gas of high oxygen pressure (10-2). The data were interpreted as indicating the presence of SO, and S,O, ions. Richardson and Fincham' have conducted the most extensive experimental study of sulfur equilibria between gas and slag. Their results confirmed many of the conclusions drawn from calculations of Richardson" and Withers. Richardson and Fincham's data fitted very well into the sulfur scheme represented by the reactions 1/2 s2 (g) + (0) melt - 1/202(g)+ (S) melt [II 1/2 S, (g) + 3/2 O (g) + (0) melt - (SO,) melt. [2] At oxygen pressures greater than 10 to 10 they found that reaction Eq. 2 was predominant while reaction Eq. 1 was controlling at oxygen pressures less than 10." to 10.". The slag compositions and gas mixtures used in their investigations were different from those used in the present study. Wherever possible, comparison has been made between their results and these, and agreement is excellent. It is evident that the distribution of sulfur between slag and gas depends upon the oxygen pressure of the gas. In FeO slags, a change in oxygen pressure produces a change in ferric oxide content, and a knowledge of this equilibrium is a prerequisite to studies of sulfur distribution. The data are found in the work of Darken and Gurry" on the FeO system and the more recent experiments of Gurry and Darken" and of Larson and Chipman" on FeO slags containing lime and silica. The effect of oxygen pressure on the ratio Fe /(Fe" + Fe ), the so-called j-ratio, reported by these investigators will be used in interpreting the results which follow. Experimental Method The purpose of the experimental program was to determine the equilibrium sulfur content in slags exposed to gases of known oxygen and sulfur pres- sures. The slag compositions selected for study were from the lime-silica-iron oxide system. Additions of magnesia were made to some of the slags. Apparatus—The apparatus used by Larson and Chipman was modified slightly to accommodate the addition of SO2 to the gas mixtures. As in their work, slag samples of 0.5 to 2.0 g were held at temperature (lcc) in platinum crucibles under a steady stream of gas, 100 to 200 ml per min, for several hours and then rapidly lowered to the bottom of the furnace where they were quenched in mercury. Preparation and Analysis of Gas Mixtures—Mixtures of SO,-CO were prepared from Virginia Smelting Co. Extra Dry liquid SO, and Pure Co. CO,. After removing traces of water vapor with an-hydrone, the CO, was passed over graphite at 1200°C, at which temperature the conversion to

Jan 1, 1957

By Gerhard Derge

THE orientation relationships resulting from allotropic transforma-tions and the formation of segregate structures in metals and alloys have been the subject of the eight earlier papers in this series1. A brief summary of orientation studies has also been given by Sachs2. A survey of these papers discloses that the factors that determine the orientation relationship of a precipitated phase to its parent solid solution, as Well as the outward form and appearance of the new phase, are not completely understood. It is now evident that crystallographically analogous systems, as a rule, exhibit the same type of Widmanstätten figure and orientation relations, so that useful information is not to be expected from examination of a new alloy involving lattice combinations of which the orientation relationships are already known. Therefore, the determina-tion of the relations existing between lattice types that have not already been studied seems to be the most promising mode of attack upon the problem; both of the systems reported in this paper represent new com-binations of lattice types.

Jan 1, 1937

By A. Vifian, I. lwasaki

Several samples of copper-nickel ore from the Duluth Gabbro were studied to relate their mineral-ogical characteristics with their amenability to concentration by flotation. The most common rocks in the samples were norites, gabbros, and troctolites. The texture of the rocks varied from coarse pegma-titic to very fine. The copper contents ranged from 0.2-0.7% and the nickel contents from 0.07-0.15%. The ore minerals were chalcopyrite, cubanite, pyrrhotite, and pentlandite. Most of the ore minerals occurred in interstices between laths of plagioclase, but some were included in the gangue grains. The samples responded readily to xanthate flotation. After a 65 to 100-mesh grind about 95% of the copper and 85% of the nickel were recovered in a bulk sulfide concentrate. Such recoveries remained constant even with grinds as fine as 270 mesh due to the extremely fine inclusions of sulfides in the silicate gangue. A finer grind than 270 mesh was necessary to free the copper-iron sulfides from the nickel-iron sulfides. A combination of time and British gum* was quite effective in producing concentrates analyzing 25-30% copper. The nickel concentrate averaged 1.5% nickel. Most of the nickel lost in the tailing was present as un-liberated sulfides and not as nickel in the olivine structure. The nickel content of the olivine was only about 0.05 or 0.08%. Western world nickel usage in 1967 is expected to be the second highest on record, amounting to 825 million lb. Despite a rise in mine production, however, demand is expected to exceed supply in 1968. ' Hence, exploration, development, and production expansion projects are being accelerated on a world scale. In Minnesota the copper-nickel bearing Duluth Gabbro is receiving much attention. During the past year 11 companies have been granted leases in the region, and the 1967 Minnesota legislature enacted a tax law designed to encourage the development of a copper-nickel industry. Although it is only during the past few years that mining companies have shown an active interest in the Minnesota copper-nickel deposit, copper-nickel minerals have been known to exist in northeastern Minnesota since 1899.3 At the 28th Mining Symposium, Dr. P. K. Sims, from the Geological Survey of Minnesota, gave a review of copper-nickel exploration in northeastern Minnesota,4 in which he emphasized that the potential of the Duluth Gabbro complex is large. Tests on samples from the Kawishiwi River area were reported by the United States Bureau of Mines in 1955.' In 1964, the Mines Experiment Station described tests on samples from the Gunflint Trail: and in 1966 the Minnesota Geological Survey published a geological map of the Gabbro Lake Quadrangle. The Mines Experiment Station published a study of the concentration of a Minnesota copper-nickel ore in 1967.7 The present paper is divided into three parts. The first describes the mineralogy of some rock samples from the Kawishiwi River area of northeastern Minnesota; the second summarizes the results of numerous flotation tests that were made on the samples, and the third explains the loss of nickel in the flotation tailing. MINERALOGY OF KAWlSHlWl ROCKS Recently five samples of mineralized gabbro from the Kawishiwi River area, a few miles east of Ely, were received at the Mines Experiment Station. One of the samples was a 175-lb composite, which was designated Ore 1556. The other four samples were 7-lb grab samples that had been obtained from four different exploration pits. They were designated Ore 1626, Lots 1 through 4. Basic Mineralogy: Many authors have reported that the rocks of the so-called gabbro of the Duluth Intrusion vary widely in composition.8-9 The samples on which our studies were based also contained a wide range of rocks. A gabbro, olivine-gabbro, anorthosite-gabbro, norite, and a troctolite were represented. The essential minerals in the samples were plagio-clase, pyroxene, and olivine, in variable proportions.

Jan 1, 1969

By Paul A. Beck

While the recrystallization properties of most of the practically important metals are known in considerable detail, those of lead are still relatively little known in spite of some valuable contributions in recent years. This condition probably is due to the difficulties involved in applying the usual methods of investigation. The microscopic method of discriminating between the elongated deformed grains of the familiar lenticular shape and the equiaxed recrys-tallized grains is not successful with fully refined lead: lenticular grains cannot be seen under the microscope with any amount of deformation whatever. The probable cause of this phenomenon was recognized long ago. With large deformation the time of recrystallization at room temperaturc is shorter than the period of preparation of the specimen for microscopic examination; with small deformation the deformed grains arc not noticeably elongated in the first place. However, with small cleformation the migration of the grain boundaries can be observed. The only systematic investigations yet published on the recrystallization of lead, those by R. S. Russell, 1-3 make use of the conditions just described. Russell considered recrystallization completed when no further migration of boundaries could be observed. A serious objection to this method arises from the fact that there is no evidence to support the view that grain-boundary migration results only from recrystallization. If such migration does result from other sources after recrystallization is completed—after the deformed grains have been replaced by new unde-formed grains—the "time of recrystallization" as determined by Russell may be too long. Furthermore, the method is subject to the above.-mentioned limitation because of the unavoidable period of preparation of the sample. According to Russell, even with the fastest technique 5 min. clapsed before the deformed samples were ready for examination, and consequently no reearystallization time shorter than 5 min. could be measured. The lack of success in detecting the recrystallization of lead by the usual hardness or tensile tests is again caused by the time necessary for

Jan 1, 1940

By Paul A. Beck

While the recrystallization properties of most of the practically important metals are known in considerable detail, those of lead are still relatively little known in spite of some valuable contributions in recent years. This condition probably is due to the difficulties involved in applying the usual methods of investigation. The microscopic method of discriminating between the elongated deformed grains of the familiar lenticular shape and the equiaxed recrys-tallized grains is not successful with fully refined lead: lenticular grains cannot be seen under the microscope with any amount of deformation whatever. The probable cause of this phenomenon was recognized long ago. With large deformation the time of recrystallization at room temperaturc is shorter than the period of preparation of the specimen for microscopic examination; with small deformation the deformed grains arc not noticeably elongated in the first place. However, with small cleformation the migration of the grain boundaries can be observed. The only systematic investigations yet published on the recrystallization of lead, those by R. S. Russell, 1-3 make use of the conditions just described. Russell considered recrystallization completed when no further migration of boundaries could be observed. A serious objection to this method arises from the fact that there is no evidence to support the view that grain-boundary migration results only from recrystallization. If such migration does result from other sources after recrystallization is completed—after the deformed grains have been replaced by new unde-formed grains—the "time of recrystallization" as determined by Russell may be too long. Furthermore, the method is subject to the above.-mentioned limitation because of the unavoidable period of preparation of the sample. According to Russell, even with the fastest technique 5 min. clapsed before the deformed samples were ready for examination, and consequently no reearystallization time shorter than 5 min. could be measured. The lack of success in detecting the recrystallization of lead by the usual hardness or tensile tests is again caused by the time necessary for

Jan 1, 1940

By W. L. McMorris, Shiou-Chuan Sun

The Convertol process was first described in Ger- many by Muschenborn1 in 1952. In the U. S. Fraser2 reported this new process in 1953, and Brisse and McMorris-resented the results of a Convertol pilot plant at the Alpheus preparation plant in Gary, W. Va., illustrating the mechanics of the process by a series of sketches. The purpose of the present investigation was threefold: 1) to determine the relative effectiveness of various oils and hydrocarbons for recovering coal by the Convertol process, 2) to ascertain the behavior of coal pulps in this process under various operational conditions, and 3) to compare Convertol with flotation in the recovery of fine coals.

Jan 11, 1959

By Clarence O. Babcock

A simple robust rock bolt load gage was tested in the laboratory to define its characteristic behavior and to obtain a measure of its performance. The gage uses three vibrating wire sensors crimped 120 (2.09 rad) apart into the outer surface of a hollow cylindrical steel, tube. The resonant frequencies of the wires change as the gage is loaded. This change is read with a Creare meter developed for the Bureau of Mines on a previous contract to read borehole stress gage results. A statistical analysis of data obtained defines the variables influencing results. A U.S. patent (3,914,992) assigned by the author to the Dept. of the Interior was granted Oct. 28, 1975.

Jan 1, 1978

By Ralph Hultgren, Prodyot Roy

Manganese vapor pressures from 1250° to 1500°K were measured by conventional Knudsen and torsion-effusion methods in twelve Fe-Mn alloys with compositions from 9 to 80 at. pct Mn. The Knudsen re-sults agveed approximately with previous measurements found in the literature which indicated the solutions were nearly ideal. However, except for the higher manganese compositions, the initial torsion readings indicated much (up to 50 pct) higher vapor presszcres than the Knudsen method. These high readings decreased steadily with time. The results are interpreted as due to depletion of surface concentration of manganese during evaporation. Thus the initial torsion readings are the most nearly correct and Knudsen methods on alloys are to be regarded with suspicion unless it can be demonstrated that diffusion rates are rapid enough to replenish surface concentrations depleted by evaporation. For the lowest manganese contents and highest temperatures, depletion causes initial torsion readings to be too low. FEW thermodynamic data are available for alloys of the high-melting transition metals due primarily to experimental difficulties at the high temperatures involved. Measurement of vapor pressure is one of the most promising techniques to be applied to this problem. From the vapor pressure of a component of an alloy phase, its activity or its partial molar Gibbs energy can be directly calculated. From measurements over a sufficient range of temperatures and compositions the partial and integral Gibbs energies, enthalpies, and entropies may be determined through Gibbs-Duhem integration. For solid phases of variable composition, which commonly are found in alloys, measured vapor pressures are low because of depletion of the surface concentration of the more volatile component as it is selectively vaporized. Diffusion from the interior tends to restore the depleted concentration. The seriousness of the effect depends on the relative rates of diffusion and vaporization. Although depletion has been recognized as a factor,' direct measurements of its rate are lacking and quantitative estimates of its effect on measurements are uncertain. In the present work the vapor pressures above a series of Fe-Mn alloys have been measured by the torsion-effusion method. This method permits a measurement of the vapor pressure of manganese as soon as the sample comes to temperature and continuously throughout the run. The rate of decline of the apparent vapor pressure measures the rate of depletion and the torsion reading at zero time should be correct. At high manganese concentrations (70 and 80 at. pct Mn), the torsion reading remained nearly constant; surface depletion was negligible. There was a slow drop in measured pressure due to bulk loss of manganese from the sample. However, for lower manganese contents, especially at high temperatures, the depletion effect was considerable and the apparent vapor pressure decreased steadily with time. For these alloys the Knudsen method should give pressures which are too low. The measurement of pressure in the Knudsen method cannot be made until enough manganese has been vaporized to be weighable. The Knudsen result is therefore an integrated average between the initial and final vapor pressures. To verify this, conventional Knudsen measurements were also made with results in approximate agreement with previously published Knudsen measurements for these alloys. As expected, for the lower manganese contents the initial torsion readings of pressure were as much as 50 pct higher than the Knudsen. THE APPARATUS The apparatus, shown in Fig. 1, is capable of operating to temperatures up to 2000°K. A vacuum of 5 x 10"6 mm Hg can be maintained. Temperatures were measured to +3° by a W-Re thermocouple placed in the dummy cell, N. The torsion cell consisted of two alumina crucibles with holes in their covers. They were placed in the molybdenum holder shown suspended from the torsion wire. Rectangular torsion wires (1 by 4 mm) were found to have superior sensitivity and less residual distortion than circular (2-mm-diameter) wires. The precision of angular measurement was found to be *0.025 deg; the variation is no doubt due to temperature fluctuation and vibration. For the Knudsen experiments the alumina cell was set on the support, N. SAMPLE PREPARATION 800-g samples were prepared by melting together electrolytic iron and electrolytic manganese and pouring the melt into a water-cooled copper mold. Melting and pouring were done under a helium at-

Jan 1, 1965

By Richard P. Gerwels

Minas de Matahambre, a copper mine located 100 miles southwest of Havana, Cuba, has produced 10 million tons of copper ore since it was first opened up in 1913. During the mid-1950's the mine was producing approximately 1000 tpd and had attained a depth of 3600 ft. As shown in Fig. 1, the property contains three shafts: the No. 1 shaft, 2100 ft deep and located 2000 ft south of the No. 2 shaft, provided service to the 2100 level; the vertical 3600-ft No. 2 shaft handled all production to the 3400 level; the No. 3 shaft on the northeasterly fringe of the mining area was in a semi-active status.

Jan 12, 1960

By Robert Glass Cleland

WALTER DOUGLAS succeeded his father, Dr. James Douglas, as president of Phelps Dodge in 1916. Before assuming office, the new president had been assayer at Bisbee, superintendent of the Copper Queen, general manager of all the Phelps Dodge mining interests, and altogether had spent a full quarter of a century in various phases of the company's business. Energetic and imaginative, experienced and courageous, he had need of all these qualities before he surrendered the direction of affairs into younger hands, fourteen years later. For the period of his administration was one of sudden ebb apd flow, flush production, drastic curtailment, quick recovery, and near-disaster. In 1917, soon after Walter Douglas became president, Phelps, Dodge & Co., Inc., which had been formed in 1908 as a holding company, went through an internal reorganization for the purpose of simplifying the structure and changing it from a holding company to an operating company. The Copper Queen Consolidated Mining Company, which had the necessary charter power and authority to carry on the business of any and all the subsidiary com-

Jan 1, 1952

By F. J. Plecity, J. T. Michalak, W. C. Leslie

W. M. Williams (McGill University)-The authors are to be congratulated on completing this detailed investigation of recrystallization behavior. The present writer has recently completed some research at the University of Toronto on the recrystallization and grain growth behavior of a number of "pure" irons, and he would like to take issue with the authors' contention that recrystallization cannot be followed by means of hardness measurements. Two series of specimens of Ferrovac E, a com- mercially available iron, were annealed to complete recrystallization at 525" and 620" C, measurements being made both of Rockwell hardness and of volume percent recrystallized as a function of annealing time. Good correlation was found between these two quantities and, following the earlier practice of Cook and Richards for copper, hardness measurements were used in an extensive investigation of recrystallization. No anomalous behavior was observed as a result of this practice. Specimens which showed complete softening always showed, (metallographically and by X-rays), completely re-crystallized structures. These observations do not, of course, detract in the least from the results of the work under discus-

Jan 1, 1962

By Peter T. Luckie, Harold L. Lovell, E. R. Palowitch, A. W. Deurbrouck, James K. Kindig

PART 1: DENSE MEDIUM SEPARATION by E. R. PALOWITCH and A. W. DEURBROUK INTRODUCTION During 1965, 64.9 percent of the 512 million tons of bituminous coal and lignite produced was cleaned mechanically, of which 95 million tons was cleaned by dense medium processes.l The percentage of bituminous coal and lignite cleaned mechanically by dense medium processes rose from 7.0 to 28.5 percent from 1938 to 1965. Dense medium separations include those coal preparation processes which clean raw coal by immersing it in a fluid having a density intermediate between clean coal and reject. As there is a general correlation between ash content and specific gravity, it is possible to achieve the required degree of removal of ash-forming impurities from a raw coal by regulating the specific gravity of the separating fluid. Dense medium processes offer the following advantages over other coal cleaning processes : 1. Ability to make sharp separations at any specific gravity within the range normally required even in the presence of high percentages of the feed in the range of e 0.1 specific gravity units. 2. Ability to maintain a separating gravity that can be controlled with ±0.005 specific gravity units. 3. Ability to handle a wide range of sizes (up to 14 inches). 4. Relatively low capital and operating costs when considered in terms of high capacity and small space requirements. 5. Ability to change specific gravity of separation to meet varying market requirements. 6. Ability to handle fluctuations in feed both in terms of quantity and quality. HISTORY Sir Henry Bessemer patented the first dense medium process in 1858. Solutions of the chlorides of iron, manganese, barium and calcium were proposed as separating liquids; the separation was made in a cone-shaped separator. One large-scale plant using calcium chloride was erected in Germany but soon was abandoned. The Chance process, using a mixture of sand and water, was first

Jan 1, 1968

By E. L. Tucker

PREVIOUS investigations of E. L. Tucker and R. E. Head' related in particular to the effect of cyanogen compounds on galena, sphalerite, and pyrite, and their behavior in the presence of such com- pounds. The present contribution deals with the float- ability of the copper minerals and of pyrite. All experiments were performed on minus 200-mesh material, the method of preparation being the same as that described in the previous article. Flotation tests were made in a small mechanically agitated machine of 50-g. capacity designed in this laboratory by Gates and Jacobsen." General Naval Stores pine oil No. 5 and potassium xanthate were used in constant amount in all of the experiments; these agents were selected because of their present wide use in the flotation of copper minerals. Lime additions were varied to secure four 'final hydrogen ion concentrations, namely, neutral, 0.0005 per cent CaO, 0.003 per cent CaO, and 0.02 per cent CaO. The variation in lime addition was introduced to include the range of alkalinities employed in actual flotation practice.

Jan 1, 1926

Wartime geological studies by the U. S. Geological Survey and subsequent drilling carried on by the Bureau of Mines disclosed new ore in the Illinois-Wisconsin zinc field. As a result, several companies are carrying on drilling programs to locate and define new ore bodies. The Vinegar Hill company, which operates a custom mill to handle ores from various sources, now employs about fifty men in production at their Andrews mine. The ore is usually found in a 200-ft horizon below the surface. Water problems are not serious. Commercial-grade ore ranges up to 8 and 9 per-cent zinc and the cut off is approximately 41/2 percent.

Jan 1, 1948