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By N. A. D. Parlee, I. D. Shah, W. C. Phelps

THIS note reports on a continuation of a program on the thermodynamics of Fe-S-X systems in the "steel-burning" temperature range begun by Bock, Barloga, and parlee.' Small coils of 0.039-in.-diameter pure iron (Ferrovac-E) wire were equilibrated with Fe-S-0 melts in ingot iron crucibles under argon at 1324°C in the assembly shown in Fig. 1, the lower part of which was heated in a large Globar furnace. Fig. 1 shows (R) the coiled iron wire sample, (M) the Fe-S-0 melt prepared from desired proportions of ferrous sulfide and ferric oxide, (K) the iron crucible, (I) a mullite guide tube, (J) an alumina crucible, (L) alundum sand, (N) crushed mullite, (Q) hollow cylinders of K30 brick, (C) a steel rod, (B), (El, (F), (G), (P), and (O), details of brass water-cooled head, and (H) a mullite tube 2-3/4 in. ID and 26 in. long. The rod (C) bearing the sample could be removed at will and be replaced by a tube for sampling the melt, or by a thermocouple for comparing the melt temperature with a control thermocouple not far from the 2-3/4-in. mullite tube. After equilibration the iron coils were treated with acid to remove the outer layer of metal and then they were analyzed for sulfur by a standard combustion method. The melt samples were analyzed for oxygen by a variation of Lander's2 hydrogen-reduction method for mattes, and for sulfur by the ASTM combustion-iodometric method NO. E 30-47. When the results of some forty-two runs were examined it was found that the sulfur and oxygen contents of the equilibrated melts showed good consistency, in that the plotted compositions fell along the smooth curve shown in Fig. 2. The points on this curve represent the experimental compositions of melts in equilibrium with ?-iron (Fe-S-0) solid solutions. These solid solutions are saturated with sulfur and oxygen with respect to the melt and therefore have the same sulfur and oxygen activities as the melt. The curve drawn through the points therefore delineates the ? liquidus. It falls in such a position as to roughly confirm the liquidus curves of Hilty and crafts3 at 1200" and 1300°C which are

Jan 1, 1965

By A. Gillis

"In order to obtain the equipment necessary to automate the equipment it was decided that the Department of Mines and Milltronics would jointly survey the circuit. This survey involved a metallurgical study by the Department of Mines and Milltronics took sound recordings during manual operation, checking in circuit bottle necks and determining the number of sensors that could be applied.The conveyer is driven by 2 PIV drives, each has a variable speed of 3/ 1. The cross conveyer that feeds directly into the rod mill feed chute will contain an automatic sampler and will eliminate the necessity of stopping the belt feeders to take samples. At present, hourly samples are taken from this point and the circuit is upset and cycling results.The Adequate scale is very close to the rod mill to totalize and thereby give a continuous indication and the second purpose is to take a signal from it and control the solution addition to the rod mill.A pneumatic positioner was obtained and put on the scale which produces a 3 tp 15 psi signal which is proportional to the actual tonnage going across the scale. This signal was fed to a bias loader which was mounted on the control panel. From there the operator can set the amount of solution that is wanted by the rod mill. No matter what the feed rate is, the signal coming from the bias loader will follow it automatically. This in turn goes to the pneumatic solution valve (1 ½” ) and the solution goes in with the feed to the rod mill. This is only part of the solution required for dilution since the rest of it is used as a force jet for the feed to the rod mill."

Jan 1, 1965

By T. E. Sterner

The Bureau of Mines investigated the use of a chromatographic gas analyzer in determining the concentration of combustion products in gas produced during field and laboratory thermal oil-recovery tests. Several parameters (carrier-gas flow, cell current, sample size, and temperature) known to affect quantitative analyses were studied using a commercially available dual-column, dual-detector chromatographic gas analyzer which had been modified to provide close control of these variables. The apparatus made possible a much closer control of air-and gas-injection rates and provided adequate data for performing material-balance calculations and for determining oxygen utilization during the laboratory and field combustion tests. The chromatographic analysis also aided materially in evaluating and measuring bypassing and gas travel times and in detecting high-permeability zones that were present in the reservoir.

Jan 1, 1965

By C J. Coveney

This paper, after a brief introduction to the mineralization and structure in the mine area, outlines the methods now being employed for grade control at Bethlehem Copper Corporation. Sampling, subgrade drilling, blasting and the actual outlining of the ore are among the topics covered. The paper concludes with a summary of the results obtained, showing a reduction in dilution and an improvement in the grade of the copper ore going to the mill. Introduction T HE Bethlehem property is located in southern British Columbia in the Highland Valley about 30 miles southeast of the town of Ashcroft. The property is located within the Guichon batholith. The rock comprising the batholith is a massive, coarse-textured diorite, which, at Bethlehem, has been intruded by a younger quartz diorite, porphyries and breccia, referred to as the "Younger Complex." Mineralization, consisting of chalcopyrite and bornite with minor pyrite and molybdenite, occurs as disseminations, fracture fillings and coarse blebs. The ore zone lies close to the Guichon -Younger Complex contact where, prior to the development of the breccia, the rocks were shattered and jointed. Subsequent mineral

Jan 1, 1965

By Haydn H. Murray

Kaolin is an important industrial mineral because it exhibits desirable properties in many applications and because of its relatively low cost, Approximately 2,000,000 tons of kaolin from Georgia and South Carolina are processed and used commercially in the United States each year. Strictly defined, the name kaolin is applied to a group of hydrous aluminum silicates of which the mineral kaolinite is the most common. Kaolinite has such desirable properties as natural whiteness, chernical stability, non- abrasiveness, and very fine particle size. Kaolinite particles are characteristically thin, flat, and hexagonal in outline. The particles range in size from submicron to as much as 40 microns (equivalent spherical diameter). In addition to the general properties mentioned in the first paragraph, it is soft, has low viscosity at high solids content in many systems, is readily wet and dispersed in water and some organic systems, and can be produced with a controlled particle size distribution. Some of the important physical constants of kaolin are: specific gravity, 2.60; index of refraction, 1.56; hardness (Mohs scale), 2; fusion temperature, 1850°C; dry brightness, 78-92 percent.1

Jan 1, 1965

By D. R. Hay, E. Scala

Electrotransport has been superimposed on the rate-limiling- step in zone refining which is the impurity diffusion through the liquid at the solid/liquid interface. The efficiency of zone refining is increased and relative resistivity ratios (P300°k/P4 2°K) he increased by 50 pel in tungsten for a given number of posses using- the electrotransport field-aided method. The effiect of zotze refining in the presence of an electric field on the relative resistivity ratio is examined as a function of its intensity and polarity. THE effect of electrodiffusion on the effective distribution coefficient of zone refining has been discussed by Pfann and Wagner.' Control of the distribution coefficient in zone refining is of twofold interest. A distribution coefficient of unity can be increased or decreased, making possible the transfer of some previously inseparable solutes. The general efficiency of zone refining can also be increased. In the conventional zone-refining process impurities are removed by their retention in the molten zone and subsequent deposition at the end of the rod after a complete passage of the zone. In higher-melting-point systems a second mechanism may also operate, the volatilization of impurities from the molten zone. It has been suggested by schadler2 that, in refractory metals, vacuum distillation plays the predominant role in purification. In Koo's results,3 the resistivity ratio decreased beyond a zone-refined length of 6 in. from the starting end, indicating that some purification does in fact occur by true zone-refining action. Hay and scala4 showed that the degree of purity as measured by the relative resistivity ratio method depends on the square root of time in the molten zone (number of passes) and thus appears to be limited by diffusion in the boundary layer at the solidifying interface assuming good mixing in the body of the molten zone where a linear rate would prevail. The final concentration of impurities in electron-beam floating-zone purification depends very much on the operating conditions and results obtained by various investigators2,3,5 are difficult to correlate. The diameter of the starting material, operating vacuum, and rate of traverse are among the factors to be considered. There are, nevertheless, some general observations to be obtained from the literature. Lawley5 reviewed the literature up to 1962 and concluded that the major contaminants generally remaining in tungsten after electron-beam zone refining are molybdenum and carbon. Molybdenum due to its high melting point and distribution coefficient of nearly unity would be expected to be difficult to remove by either volatilization or zone refining. Carbon is not only a common contaminant in vacuum systems, but is also very difficult to remove by conventional vacuum melting. even with vacuums of 10-7 mm Hg. For each of those impurities removed by zone refining the equation of Pfann and Wagner may be applied: It relates the effective distribution coefficient k to a superimposed driving force which accelerates the solute away from the interface with a terminal velocity L" and to the more conventional zone-refining parameters; v = rate of traverse, t = thickness of the diffusion layer at the solidifying interface, D = diffusivity of the solute in the molten zone, and ko = equilibrium distribution coefficient of the impurity.

Jan 1, 1965

By A. H. Daane, W. J. Wunderlin, B. J. Beaudry

In an earlier study at this laboratory,' the authors investigated the solid solubility of holmium in copper, silver, and gold, and also the melting point of the first eutectic on the noble-metal-rich side in these systems. In a more recent study of the solubility of rare-earth metals in gold at this laboratory. Rider, Gschneidner, and McMasters2 noted that the reported eutectic temperature in the Ho-Au system was lower than the corresponding eutectics in systems of dysprosium and erbium with gold. A redetermination of the eutectic temperature in the Ho-Au system with the same alloy used in the original study showed the eutectic temperature to be 810°C instead of 778°C as originally reported. (The eutectic temperatures in the Ho-Ag and Ho-Cu systems were also redetermined and were found to be 795" and 864°C compared to 787° and 868°C, respectively, which were reported originally.) Since this large change in eutectic temperature made the solubility data appear questionable, new alloys were prepared, heat-treated, and examined metallographically. The procedure of sample preparation and heat treatment used in the original work' was followed except longer heat treatments were used ranging from 7 days at 600°C to 6 hr at 900°C. The results obtained are shown in Fig. 1. There is good agreement between the two studies in the maximum solubility of holmium in gold. Since the slope of the solvus is less pronounced in the present study, the extrapolation to 550°C shows a solubility of 1.6 wt pct Ho in gold compared with 1.0 wt pct in the original work. Since additional data were obtained and longer heat treatments were used in the present study, the larger value is believed to be more accurate. The authors wish to express their appreciation to P. Rider and K. A. Gschneidner. Jr., for bringing this discrepancy to their attention, and also to D. Thompson for assisting in the present study.

Jan 1, 1965

By A. J. Forney

Recent experiments used catalysts of plate assemblies in synthesizing high-Btu gas and gasoline indirectly from coal. A gas with a heating value of 925 to 943 Bt-: per cubic foot has been prod u la the hot-gas-recycle pilot plant from synthesis gas (3H2+100) with lathe turnings used as catalyst in the first reactor, and assemblies of parallel sprayed plats of nickel in the second. Solid plates made of Raney nickel, and steel and aluminum plates sprayed with Raney nickel or nickel oxide were tested. Those catalysts had very low resistance to gas flow; 90 percent lower than nickel granules used in previous experiments. In a single stage of synthesis thee nickel plates were only partially successful. Although the heating values of the product gas ranged from 856 to 941 Btu per cubic foot, the carbon monoxide content of he gas was above 0.1 percent. Both steel and wrought turnings were tested in single-stage synthesis, but the conversion of hydrogen and carbon monoxide was too low to attain the desired heating value of 900 Btu per cubic foot in the product gas. Assemblies of plates thermally sprayed with fusel iron were tried in an experiment to make gasoline. A gasoline yield of 52 percent (of the hydro¬carbons produced) was obtained using a 1H2-10O feed These sprayed assemblies were in service for 1,500 hours, the longest that this type of catalyst has been used. When a second reactor containing Raney nickel catalyst was added in series with the first reactor, complete utilization of the feed gas was obtained because in addition to the liquid product, a high-Btu gas with a heating value of 800 Btu per cubic foot was made.

Jan 1, 1965

By B. E. Eakin, A. L. Lee

Atmospheric pressure viscosity values For light hydrocarbons were calculated by a simple mixing rule based on the Sutherland constants for pure components. This method was further extended so that the atmospheric pressure viscosity of a mixture may be calculated based on the molecular weight information only. INTRODUCTION A proven method for estimating the gas-phase viscosity of a mixture is the one by Herning and zipperer.l This mixing rule has the following form: One method for calculating the pure component viscosity i is the Sutherland equation,2 which has the following form: The Sutherland constants B and S are determined from experimental data. A set of Sutherland constants for light hydrocarbons based on the data of several investigators3-5 is presented in Table 1. APPLICATION The Herning-Zipperer equation and the Sutherland equation were used to obtain an equation for calculating the gas-phase viscosity of light hydrocarbons. This equation has the form, Eq. 3 was used successfully in the study of methane-n-butane mixtures.6 Further analysis indicated that the Sutherland constants are a function of molecular weight.7 The gas-phase viscosity may be calculated based on molecular weight information only. The following equation was developed: The atmospheric pressure viscosity of ethane, propane, n-butaneand four methane-propane mixtures calculated on the basis of Eq. 6 are compared with the data of other investigators in Tables 2, 3, 4 and 5, respectively. A plot of atmospheric pressure viscosity vs molecular weight based on Eq. 6 is presented in Fig. 1.

Jan 1, 1965

By Richard L. Ash

In many instances, blasting exerts the dominant control over the economics and safety of excavation, where the materials involved are too hard and tough to be fragmented efficiently by other means. However, associated with the fragmentation process other effects very often result that are not desirable and may even be hazardous, such as fly rock, air blast, excessive overbreak, and damaging ground virbrations. It has always been the desire of those concerned with blasting to better control the forces involved so as to improve the breakage of materials, but at the same time reduce, or eliminate if possible, the unwanted side effects. Until the last decade or two, little was known of the phenomena concerned with blasting. However, since that time many investigators have studied blast mechanisms produced from both chemical and nuclear explosions, with the result that general concepts of the principles have been developed. But, in general, it is assumed that the energy from the explosion would be propagated spherically throughout the material, the latter of which for convenience of analyses is considered homogeneous and isotropic, i.e., the properties are the same in all directions, However, rocks are not isotropic as a rule, and evidence clearly indicates blasting forces rarely function uniformly or in spherical form as theorized.

Jan 1, 1965

By Roger N. Dokken

It is well-known1-4 that Fe-Si alloys from approximately 9 to 27 at. pct Si show an ordered structure of the Fe3Si type at room temperature. Recently Meinhardt and Krisement,' through an investigation of Fe-Si alloys at room temperature by neutron diffraction, discovered that at 10.8 at. pct Si ordering of the FeSi type occurs while above this composition the normal Fe3Si-type superstructure appears. This FeSi type of ordering was also found by Davies8 as indicated by X-ray diffraction measurements on an Fe-8.7 at. pct Si alloy. Meinhardt and Krisement7 extended their neutron-diffraction work and determined the phase-boundary temperatures for both FeSi- and Fe3Si-type ordering. Ordering phenomena can also be studied by resistance measurements.4,8-11 Krivoglas and Maty-sina" carried out a theoretical development of the

Jan 1, 1965

By C. E. Morris, S. R. Pollack

Current -vo1tage -temperature characteristics were studied for Al-A12O3-Al, Au structures. The oxide film was grown by gaseous oxidation in an 0, glow discharge. The electron-transfer mechanism was identified as tunneling and the barrier heights and thickness were determined. It was found that the barrier height at the parent aluminum-oxide interface is 1.5 ev and the built-in vloltage with an aluminum counter electrode is 0.35 v. The growth mechanism of the oxide is also discussed and it is suggested that Mott&apos;s theory is not applicable in describing the growth. Discrepancies were observed in the detailed comparison of tunneling theory, based on a trapezoidal model, with the data, and several possible explanations are discussed. THEORETICAL analyses of electron tunneling from one nonsuperconducting metal to another through an extremely thin insulating film have been presented.1-6 These calculations relate the current density, J, to the voltage, V, between the two metals, and to the temperature, T. The results of these calculations indicate that the magnitude of J and the detailed shape of the J-V characteristic will in general depend most strongly upon such properties of the insulating film as the thickness, the dielectric constant, and the structure of the electron energy barrier profile. The experimental results of many7-11 workers have corroborated the main features of these calcu- lations and have in fact been used to determine properties of the thin insulating film. It has been demonstrated, for example, that the tunneling current formulation of simmons4 is adequate to describe the observed J-V characteristic over approximately 10 orders of magnitude of current. Furthermore, from these observations and analyses, insight into the nature of the A1-A12O3 (thermally grown) interface region has been obtained.&apos;&apos; The temperature dependence of the tunnel current has also been studied and, although a self-consistent set of tunneling parameters can be chosen to describe these data at low voltages (i.e., <0.5 v), the tunneling parameters are different from those obtained from higher voltage (i.e., of the order of 1 to 5 v) measurements." We have measured the effect of temperature and voltage upon the tunnel current at higher applied voltages and find that the theory is inadequate to describe all of the effects reported here. A discussion of the origin of this inadequacy is presented following a description of the samples used for these experiments, and the experimental results. SAMPLE PREPARATION Metal-insulator-metal structures were fabricated in the following way. A 99.999 pct A1 charge was used to deposit, in vacuo, thirty films, 2000Å thick, onto a 1 by 2 in. glass substrate (7059 Corning glass). Prior to deposition the substrate was glow-discharged for final cleanup and then baked at 200°C for 2 hr at a pressure of 5 x 10-7 torr. The pressure during deposition of the metal films was 2 X 10-6 torr and the deposition rate was 50 to 100Å per

Jan 1, 1965

By F. W. Jessen, H. Kazemi

A washing technique has been developed to form a spherical cavity in massive salt. The technique is, basically, a process of controlling the fluid motion in the cavity, the concentration distribution of brine, the rate of dissolution at the walls of the cavity, and the particular settings of the wash pipe, or pipes (inlet and outlet pipe) employed. For a particular arrangement of tubing and casing, fresh water enters from the casing annulus at a position above the bottom of the tubing, and the dissolved material leaves the cavity through the tubing near the bottom of the projected hole. The initial configuration of the cavity is cylindrical, representing the drilled hole situated at the axis of the projected cavity. As washing progresses the original hole is enlarged radially (any direction perpendicular to the axis of the hole). An inert fluid (generally a hydrocarbon, natural gas, or air) which serves as a blanket is injected through the annular space between the original hole and the casing. The controlled downward motion of this blanket maintains the upper edge of the brine region that is expanding on the surface of the projected sphere. A large spherical glass container and a radial model were used to investigate the flow patterns and the concentration distribution of brine occurring during the progress of solution of the salt. Aluminum flakes and dye were injected and flow patterns were observed and recorded on motion picture film. Based on the results of these model studies and other work carried out in this laboratory, the controlled washing technique was formulated. INTRODUCTION Underground cavities leached in salt beds and salt domes have been used extensively for storing hydrocarbons. Little attention has been focused on the shape of the cavities as long as large volumes were obtained and the cavities were structurally stable. The general process involves circulating fresh water and removing brine. Two distinctly different circulating systems can be employed, each of which yields characteristically different shapes. By far the most generally accepted method of washing storage caverns in salt domes is the direct circulation system. Water is introduced through the innermost pipe of a concentric pipe system, and brine is withdrawn through the annulus. In the reverse-circulation method, water enters through the annulus and is discharged through the smallesc tubing string. The size of the operation, and hence the size of tubing and casing used, depends on such factors as cavity volume, length of hole, availability of water, disposal of brine and power requirements. Underground caverns are from 100 to 1,000 ft or more in length, and when completed vary from 40 to 100 ft in diameter, providing storage of 100,000 bbl or more. The volumes of water required per volume of salt removed vary from 6 to 7 for the reverse circulation method to 10 to 11 for the direct circulation method. Up to 80,000 BWPD are often circulated. In the direct circulation method, because water enters near the bottom of the projected cavity, solution of salt is greatest at this point, particularly in view of the fact that when the washing is begun turbulent flow undoubtedly exists in the immediate vicinity of the discharge of the inlet water. As the diameter of the hole increases, flow rates also are increased, so perhaps the condition of fluid turbulence is maintained for some time. During the later stages of leaching, when capacity of equipment may be the limiting factor in maintaining flow rates, there may still exist some turbulence adjacent to the point of influx; however, for the most part laminar flow conditions prevail. There appears, therefore, rather good evidence to indicate that the state of fluid motion is responsible for the typically shaped cavity which results from such washing — namely a cylindrical form, generally somewhat larger at the bottom than at the top. Depending on the number of so-called stages which might be employed, the walls or surfaces of the salt diminish rather uniformly from bottom to

Jan 1, 1965

By J. W. Taylor, E. G. Zukas

THE results of shock-loading studies on copper were reported several years ago by smith. In his experiments, Smith found that there was a correlation between the shock direction and the orientation of twins which the shock produced. By using free-surface-type shots in which the free surface of the specimen was not normal to the shock direction, he showed conclusively that twinning of copper in impulsive loading was caused by the rarefaction wave. Similar tests with iron, however, showed that it twinned during compression. More recent studies of iron2 and on Fe-Si single crystals3 have shown that twinning can be suppressed in these materials by shock loading at pressures high enough so that the velocity of the shock wave exceeds the elastic-wave velocity. From these observations, it appeared that twinning was caused by the shear stresses present in the zone undergoing adjustment from one-dimensional to three-dimensional loading. At high pressures, such a zone becomes so thin that there is insufficient time for the relatively ordered motion of atoms involved in twinning to occur. Twinning in copper, therefore, cannot be produced by a single compressive shock wave because resolved shear stress large enough to create twins exists only for a very short time (0.01 psec or less) before the pressure increases suddenly and loading becomes essentially hydrostatic. (A typical pressure vs time record for a copper shot, illustrating the short rise time of the compression wave, is shown in Fig. 1.) If, on the other hand, a second shock wave can be created in a precompressed sample, then the new elastic limit is several kilobars,4 and a resolved shear stress sufficient to cause twinning should be maintained for an adequate time period (0.1 psec or more). This experimental situation can, in fact, be realized. The experimental arrangement used to do so is shown in Fig. 2. By utilizing the pressure transformation in Fe-V alloys, it was possible to shock-load the copper in compression while the copper was already precompressed. In the first test, an 8 wt pct V-Fe sample was used as a driver for loading the copper, and the copper was exposed to the following series of compressive shocks: 1) an elastic wave of about 8 kbars, which is usually ignored in shock studies; 2) the pressure transformation wave for the driver of 200 kbars; and 3) the driving shock wave of 270 kbars pressure. Metallurgical determination of the angular twin distribution, shown in Fig. 3, with respect to the shock direction and the shock rarefaction direction (which was 23 deg from the shock direction) showed that twinning took place

Jan 1, 1965

By R. D. Daniels, T. W. Wood

The tensile properties of columbium and Cb-H alloys containing up to 455 ppm H were studied as a function of temperature and strain rate. Hydrogen, introduced into columbium at elevated temperatures, using a thermal -equilibrium technique, embrittled columbium most severely at about —77°C. This elnbrittle ment occurred even at hydrogen concentrations of an order of 20 ppm. At higher temperatures, the hydrogen tolerance of columbium increased in relation to the increased solubility of hydrogen in tile metal. Below this temperature hydrogen tolerance, as determined by ductility and fracture stress, increased slightly. Strain rate had little effect on the tensile results for cross-head speeds over the range 0.002 to 2.0 in. per min. Strain aging during the tensile test appears to explain the ductility mininmum at —77°C. The apparent increase in hydrogen tolerance at lower temperatures is attributed to the low mobility of hyhogen. Experiments were performed in which samples were prestrained in tension at room temperature and tested to failure at —196°C. Results suggest that hydrogetz segregation to preformed crack nuclei can cause subsequent embrittlement even at temperatures where hydrogen mobility is too low to cause embrittlement in a normal tensile test. COLUMBIUM is an example of the class of bcc metals with ductile-brittle transition temperatures sensitive to the presence of interstitial atom contaminants. Hydrogen is one of these embrittling contaminants. The embrittling effect of hydrogen is less potent, perhaps, in columbium than in some of the other bcc refractory metals, but it is still a problem of both theoretical and practical interest. Unlike hydrogen in iron and steels, hydrogen in columbium is exothermically rather than endo-thermically occluded. The embrittlement process in exothermic systems has not been studied as extensively as that in endothermic systems, especially at hydrogen concentrations below the limit of solubility. The purpose of this investigation was to evaluate the embrittlement process in initially pure columbium as a function of hydrogen content, temperature, and strain rate. The Cb-H phase diagram, according to Albrecht et al.,1 is shown in Fig. 1. Columbium reacts exothermically with hydrogen producing a solid solution at concentrations of less than about 250 ppm (parts per million by weight) H at room temperature. At concentrations above the highly temperature-dependent solvus a second phase is formed. Like many similar hydrogen-metal systems,2 his system exhibits a miscibility gap with respect to hydrogen solution. Albrecht found the critical temperature of the miscibility gap to be about 140°C, the critical concentration to be 0.23 atom fraction hydrogen, and the critical pressure to be 0.01 mm Hg. Above 140°C there is a solid solution of increasing lattice constant extending across the phase diagram. Hydrogen concentrations of particular interest in this investigation were those below the limit of solubility in columbium. At hydrogen concentrations above the limit of solubility, columbium will contain the hydrogen-rich second phase and will be brittle under most testing conditions because the hydride generally precipitates as platelets with coincident matrix lattice strains.1&apos;3 At hydrogen concentrations below the limit of solubility, the tensile behavior of columbium is expected to be more sensitive to the interrelationships between hydrogen concentration and mobility and the testing variables such as temperature and strain rate. Literature references to the hydrogen embrittlement of metals, especially ferrous alloys and titanium alloys, are too voluminous to mention. It is only recently, however, that detailed studies of the hydrogen embrittlement of columbium have been undertaken. Wilcox et a1.4 studied the strain rate and temperature dependences of the low-temperature deformation behavior of fine-grained are-melted columbium (1 ppm H) and the effect of hydrogen content (1,9, and 30 ppm H) on the mechanical behavior of columbium at a series of temperatures for a single strain rate. A strain-aging peak was ob-served at about -50°C which was attributed to the presence of hydrogen in the metal. Eustice and carlson5 studied the effect of hydrogen on the ductility of V-Cb alloys at a series of temperatures over the range -196° to 25°C. Pure columbium was embrittled by 20 ppm H which produced a ductility transition at approximately -70°C. Ingram et al.6 studied the effect of oxygen and hydrogen on the tensile properties of columbium and tantalum. A minimum in the notched-to-unnotched tensile ratio of hydrogenated columbium was obtained at about -75°C, but because of the relatively large hydrogen content employed (200 and 390 ppm) the ductility

Jan 1, 1965

By A. J. Hatch

Recent disclosures concerning strengthening of anisotropic sheet materials under biaxial stresses are reviewed. This biaxial strengthening has been termed "texture hardening" by Backofen and is related to the normal anisotropy parameter, R. Measurements of R made on three annealed titanium alloys indicate a Ti-4Al alloy will have the greatest potential for texture hardening, followed in order by Ti-5Al-2.5Sn and Ti-6Al-4V. Relative to sheet texture, a review of the deformation mechanisms in titanium alloys would indicate that a preferred orientation for "texture hardening" is where the (0001) pole is normal to the sheet plane. This was confirmed by determination oj (0001) pole figures for the above three alloys. High R values are related to pole figures with (0001) normal to the sheet plane, whereas low R values are related to pole figures with (0001) split in the transverse direction from the sheet normal. PUBLISHED work by Backofen et al. 1 and Hosford and Backofen2 based on hill&apos;s&apos; mathematical theory of yielding in anisotropic metals has indicated that significant strength advantages under biaxial stresses are possible in hcp alloys, provided an ideal (0001) [1010] sheet texture exists. This tendency to strengthen under biaxial stresses has been termed "texture hardening".1 It can be quantita- tively characterized by a strain-ratio parameter, R, where R may be determined from the ratio of natural width strain to natural thickness strain as measured on a uniaxial test specimen cut parallel to the rolling direction. If R is greater than 1.0, then strengthening under biaxial tension would be predicted. Considering the a titanium alloys which have an hcp crystal structure, Williams and Eppelsheimer4 have reported that commercial-purity grades deviate from the ideal (0001) sheet texture mainly in an approximate 30-deg rotation of the basal plane, toward the transverse sheet direction. However, McHargue et a1.5 have shown that the angle of rotation of the basal plane is sensitive to alloy content. In particular, a titanium alloy with 3.8 pct Al was reported to have the ideal (0001) [1010] texture after cold rolling. Additionally, Backofen et a1.1 using plane-strain compression tests have reported R values greater than 5.0 for the commercial 0 alloy Ti-5A1-2.Sn (110-AT). In view of these findings, a program was initiated to further determine the potential of commercial Ti-5A1-2.5Sn and an experimental Ti-4A1 alloy with respect to "texture hardening". Also, because of its wide commercial use, Ti-6A1-4V was included in the investigation. BIAXIAL-STRESS THEORY FOR ANISOTROPIC MATERIALS Backofen ef al.,1 based on the mathematical theory of Hi11,3 has introduced the concept of "texture hardening". In this work, it was shown that possi-

Jan 1, 1965

By Richard D. Miller

This publication contains routine analyses and related source data for 295 natural gas samples from 18 States collected during calendar year 1963 as part of a continuous survey of the United States for occurrences of helium in natural gas. This survey has been conducted by the Bureau of Mines since 1917. The analyses published herein were made by mass spectrometer and a special helium analysis apparatus, which are described in Bureau of Mines Bulletins 4863/ and 576.4/

Jan 1, 1965

By R. A. Fitch, J. D. Griffith

A performance calculation method was used in conjunction with experimental studies to develop means of predicting and interpreting miscible floods and to explore possible methods. of improving their efficiency. The calculation method is based upon the division of reservoirs into multiple independent zones or strata. Comparison was made with some experimental floods and with a field project to obtain some measure of the applicability of the method. Two aspects of miscible flooding were considered: (I) the displacement of a miscible front through a reservoir, and (2) the distribution and utilization of the solvent volume injected to maintain miscibility. Calculations and experihental observations indicate that alternate gas-water injection behind a miscible front significantly improves miscible flood performance, both within a single stratum and in a multistrata reservoir. Calculations were made on the extent to which miscibiliry is maintained by a given solvent volume in a stratified reservoir. Two alternate criteria for determining the optimum volume of solvent for injection are discussed. The preinjection of a small volume of water ahead of the solvent is suggested as a method of obtaining more efficient utilization of solvent. Calculations and experiments were made to investigate the effects of water preinjection. INTRODUCTION Miscible fluid displacement as a possible means of recovering oil has been the subject of extensive research and numerous field tests over the past several years. This work has brought out both favorable and unfavorable features of the miscible recovery methods. Many tests have shown that a miscible fluid can displace all of the oil contacted, leaving no high residual oil saturation, as is characteristic of immiscible displacements. The miscible methods have proven dificult to control, however, as evidenced by early breakthrough of the displacing fluid and poor sweep efficiency in several field projects. It became apparent early in the investigation of miscible displacement that the development of improved techniques and better methods of control would be required to extend the range of applicability to any significant portion of our petroleum reservoirs. The purpose of this study was to consider the problem of designing miscible floods to obtain better performance. A performance calculation was used in conjunction with experimental studies to develop means of predicting and interpreting miscible floods and to explore possible methods of improving their efficiency. Two aspects of miscible floods were considered separately in this study and the results are presented in two parts. The first part concerns the manner in which the miscible front is displaced through the reservoir. In these calculations the condition of miscibility between the reservoir oil and the displacing fluid is assumed. In the second portion the distribution and utilization of the preinjected solvent in maintaining rniscibility is considered. This portion dealing with solvent utilization applies only to the enriched gas or LPG slug processes. CALCULATION METHOD AND EXPERIMENTAL STUDIES COMPUTATIONAL MODEL The calculations for expected reservoir performance are based upon the multi-strata concept of reservoir properties. The method assumes multiple, independent strata (no crossflow between strata) and explicitly includes variations in patterns, injectivity, areal sweep and displacement efficiency. Lateral variation in permeability within the strata (for example, directional permeability) may be considered in the calculations, provided the variations are similar in all strata. The calculations based on this model furnish the rates of injection and rates of production of both oil and the displacing fluid for the composite system of strata. To carry out calculations on the mathematical model described, information is required on the performance of the displacement process under consideration in a single stratum element of the pattern to be used. In particular, for a given pattern and displacement process, data are required relating injectivity and composition of the produced stream to the volume of fluid injected. Data on the variations in areal sweep must also be available if it is desired to track the areal sweeps in the multi-strata model. These data may be obtained from experimental work such as model studies or other suitable methods. This representation of reservoir properties is, of course, an approximation and may be inappropriate in some cases. But the representation is not an arbitrary one since most oil reservoirs are essentially successive layers of sediment with the net producing pay zone often comprising but a fraction of the gross formation thickness. The fact that permeabilities measured in the vertical direction are frequently but a fraction of the horizontal permeability adds some evidence to the validity of this model. This type cal-

Jan 1, 1965

By C S. Stevens

This paper describes the problems encountered and the steps taken to solve them in milling an ore containing relatively large amounts of pyrrhotite. A complex and greatly lengthened flotation circuit was required to recover the pyrrhotite. A very low pH had to be maintained in the cyanide circuit in order to get good recovery of the gold and maintain reasonable cyanide recovery. Introduction D ELNITE Mines Ltd., a gold mine situated about 5 miles by road south and east of the town of Timmins, Ontario, is serviced by two shafts. No. 2 shaft extends from surface to the 2875-ft. level, and No. 3 shaft, an internal winze, extends from the 2875-to the 5275-ft. level. No. 2 shaft was stopped at the 2875-ft. level because of a heavy band of chloritic schist which necessitated a drive to the north for 1000 feet, where No. 3 shaft was sunk. The latter bottomed in the schist at the 5275-ft. level. From the 2500 to the 2875-ft. level in No. 2 shaft, the ore was

Jan 1, 1965

By Atmaram H. Soni

A statistical study of machinability led the writer to examine existing data in regard to a thermal conductivity-mechanical properties relationship. Various functional relationships were proposed and the multiple correlation determined by statistical methods discussed in detail in the 1iterature.4 The relationship having the greatest engineering and statistical significance is discussed below. The data for cast and wrought aluminum alloys&apos;&apos;2 have been compiled and analyzed separately. The results of these analyses are presented in Table I. The empirical equations for estimating the thermal conductivity (cal sec-&apos; cm-I °C) are: for cast aluminum alloys K = 0.584 -0.00984/ -0.00263 Hb [1] and for wrought aluminum alloys K = 0.604 -0.00424l- 0.00170 Hb [2] where 1 and Hb are the percentage elongation and Brinell hardness number. Results of a similar analysis pertaining to stainless steel3 are also given in Table I. This empirical equation for estimating thermal conductivity (Btu per sq ft per hr per °F per in.) is K = 216.19- 1.716l - 0.0997 Hb [3] The relationship between electrical resistivity and mechanical properties was also examined for aluminum alloys using the same statistical method. These results are listed in Table II. While the situation of exact multiple correlation

Jan 1, 1965