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By d&apos, K. Mukherjee, C. R. Antonio, R. J. Maciag, G. J. Fischer

Tensile data indicate that over the range of strain rates 10-5 to 10-1 sec-1 and in the temperature range 298° to 743°K the flow stress at a given temperature may be expressed as: C0 = Cem where m changes abruptly at a critical strain rate of 10-2 sec-1. The Zener-Hollomon parameter was tested and found to be invalid except at temperatures exceeding 700° K. Values of AH calculated for temperatures above 700°K ranged from 30 to 47.5 kcal per g-mole. ThE flow characteristics of aluminum and aluminum alloys as a function of temperature and strain rate have been of interest to various experimenters for many years. Trozera et al.1 determined tensile flow curves for pure aluminum and concluded that the combined effect of temperature and strain rate on the flow stress could be related using the Zener-Hollomon parameter. More recently, Hockett2 proposed a relationship between compressive flow stress, temperature, and true strain rate which could be represented by a surface. Holt et al.3 studied strain rate effects on flow stress in a number of aluminum alloys at room temperature. It was determined that there is a critical strain rate above which a strain rate effect is observed. It was also reported that the strain rate sensitivity was significant in aluminum alloys in the "0" condition only. In a recent review paper McQueen4 has considered a number of mathematical expressions which have been used to describe the relationship between stress, strain rate, and temperature. These expressions have been applied to the flow characteristics of a number of different metals and alloys including aluminum. In the present work the strain rate sensitivity of 7075-0 aluminum was determined in the temperature range of 298° to 743°K. The tensile flow stress at 0.2 pct offset was obtained over a nominal strain rate range of 10-5 to 10-1 sec-1. EXPERIMENTAL Threaded tensile specimens were cut from a single heat of 7075-T6 aluminum. The composition of this heat is given in Table I. The test bars had a gage section 1.5 in. long by 0.250 in. diam and conformed to ASTM specification E-8-57T. After machining, the bars were annealed at 413° ± 10°C for 2 hr. They were then cooled to 260°C in 3 hr, and finally air cooled to room temperature. This treatment is commonly used to produce the "0" condition. Load-time curves at constant crosshead speeds were obtained at various temperatures using an Instron testing machine. Crosshead speeds ranged from 0.002 to 40 in. per min. A three-zone resistance tube furnace was used for the elevated-temperature tests. Temperatures were measured at three points along the gage length by means of suitably placed thermocouples. Each tensile bar was held at temperature for 30 min prior to testing and the maximum temperature variation along the gage length was kept below 1°C. In all, 275 samples were tested and each data point plotted is an average of at least two tests. In many cases the point represents up to six tests. RESULTS AND DISCUSSION Values of the flow stress at 0.2 pct offset at six different temperatures are plotted vs strain rate on log-log coordinates in Fig. 1. Over discrete ranges of strain rate, the data for each temperature fit the expression:

Jan 1, 1969

By R. C. Earlougher, F. G. Miller, T. D. Mueller, H. J. Ramey

There are many studies of flow in radial systems that can be used to interpret unsteady rerervoir flow problems. Although solutions for systems of infinite extent can be used to generate solutions fur finite ow systems by superposition, application is tedious. In this paper a step is made toward simplifying calcu1ations of such solutions for finite flow systems. Superposition is used to produce a tabulu-lion of the dimension1e.s.s pressure drop function at several locations within a bounded square that has a well at its center. The square system provides a useful building block that may be used to generate flow behavior for any rectangular shape whose sides are in integral ratios. Values of the tabulated dimensionless pressure drop function are simply added to obtain the dimensionless pressure drop function for the desired rectangulm system. The rectangular system may contain any number of wells producing at any rates. Furthermore, the outer boundaries of the rectangular system may be closed (no-flow) or they may he at constant pressure. Mixed conditions also may be conyidered. Tables of the dimensionless pressure drop function for the square system are presented and various applications of the technique are illustrated. Introduction In 1945, van Everdingen and Hurst' published solutions for the problem of water influx into a cylindrical reservoir. Since this problem is mathematically identical with the depletion of a cylindrical reservoir with a well at the origin, the van Everdingen-Hurst solution may be used to study the depletion problem. In their analysis, they assumed that the fluid had a small, constant compressibility such that flow was governed by the diffusivity equation For a constant production rate q starting at time zero, van Everdingen and Hurst showed that the unsteady pressurc distribution for both finite and infinite systems could be expressed in terms of a dimensionless pressure 'Sabulations of the dimensionless pressure drop for a unit value of r, were provided by van Everdingen and Hurst,' and later by Chatas.' Others also presented values in graphical or tabular form." If the radius of the well becomes vanishingly small, r,+ O, the line source solution may be used for Eq. 2 when infinite systems are considered. Eqs. 5 and 6 are excellent approximations for Eq. 2 under certain conditions: In 1954, Matthews, Brons and HazebroekV emonstrated that solutions such as Eq. 5 can be superposed to generate the behavior of bounded geometric shapes; i.e., the behavior of a bounded single-well system can be calculated by adding together the pressure disturbances caused by the appropriate array of an infinite number of wells producing from an infinite system. These wells are referred to as image wells. Matthews, Brons and Hazebroek considered systems containing a single well producing at a constant rate. This superposition can be represented analytically as

Jan 1, 1969

By Harrison R. Cooper

Computer process analysis and control techniques are overcoming major hurdles to acceptance in the mineral industry. With the growing list of new advances characteristic of a rapidly maturing discipline, management of the companies on the leading edge are keenly aware of the advantages of using computer methods in process applications. Significant advancement is already evident in such technical areas as operations research, mathematical modeling, statistical methods, and computer-based procedural techniques. The early advances during the past decade are already documented in prior symposium proceedings of this series. Thus, the currently active areas of the advancing technology are emphasized here. This section deals with applications in pyrometallurgical and kiln processes. The two sections which follow deal with concentrating operations from two points of view: 1) mathematical modeling, and 2) on-line control. In the metallurgical field, emphasis on developing effective process computer applications for the steel industry began in the late 1950's. Simulation techniques also received substantial attention. The steel industry was soon joined by the cement industry in the development of computer methods for process applications. Computers were in use for feed-material blending and kiln control in the early 1960's. Computer development in other pyro processes, such as aluminum reduction and glass-making, also marked significant advances by the mid 1960's. Aluminum smelter potline control is a nearly universal application at this point, and the development of glass furnace computer process control represented a recent important technical advance in digital control techniques. Steel Hot strip rolling was the earliest significant process computer application in the metallurgical industry. Computer control of rolling mill operations is now a steel mill standard component, particularly in plants newly placed into production. 1, 2 Initial computer installations principally carried out procedural routines in setting mill clearances for production lot control. Recent developments are leading toward feedback control based on mathematical model techniques. 3

Jan 1, 1969

By W. C. Coons, E. H. Rennhack, R. A. Perkins

THE constitution of Ti-N alloys containing up to 17.5 wt pct N has been investigated by Palty, Margolin, and Nielsen.1 Their results, which confirmed earlier work

Jan 1, 1969

By S. R. B. Cooke, S. W. Clark

Adsorption of calcium and magnesium by quartz was determined over a wide pH range using flame photometry for solution analysis. A parallelism was noted between calcium adsorption at alkaline pH and flotation of activated quartz by means of various fatty acid collectors. Abstraction of calcium from 100 ppm solutions increased above pH 10.5 until all of the calcium was removed at pH values between 12 and 12.5. Calcium was desorbed from the quartz over the pH range 12.5 to 13.0 and returned to the solution. Precipitation of magnesium hydroxide prevented measurement of magnesium adsorption above a pH of 9.9. A calcium adsorption isotherm determined at pH 9 matched measurements of barium adsorption by other investigators over the range where adsorption corresponded to the equation of a Freundlich adsorption isotherm. In accordance with the Gouy-Chapman theory for adsorption in the diffuse layer, adsorption of the divalent cations under these conditions was four times the adsorption of monovalent sodium. Activation of quartz by multivalent metal cations in flotation using anionic collectors has been studied by many investigators. The occurrence of activator cations in the water of flotation mills makes depression of silaceous gangue very difficult. Alternatively, in some flotation systems it is practical to cause activation of quartz so that it is floated from the desirable mineral values. The present study was initiated to investigate the activation of quartz by measuring adsorption of calcium and magnesium ions as a function of solution pH. Early empirical tests showed that quartz would be activated to flotation using anionic collectors if any of a number of divalent or trivalent metallic cations were present in the pulp.1*2 Subsequent studies by Clemmer,3 Cooke and Digre,4 Cooke,5 Schuhmann and Prakash,6 and Cooke, Iwasaki, and Choi,7-8 showed that flotation depended strongly upon the alkalinity of the flotation pulp, the concentration of the activating cations, and the chain length and structure of the organic collectors used. The concept of the electrical double layer has been applied to the case of the quartz-aqueous solution interface by Gaudin and Fuerstenau,9-10 and by de Bruyn 11 to explain the activation of quartz by multivalent metal cations. Studies of the surface of quartz by Gaudin and Fuerstenau9,10,12 and by Li " using the streaming potential technique contributed much information on the electro kinetic condition of the surface of quartz in the presence of various organic and inorganic ions. Measurement of adsorption of ac-

Jan 1, 1969

By R. L. Skaggs, D. T. Peterson

The effect of carbon in solid solution on the plastic behavior of thorium was studied by measuring the flow stress of Th-C alloys from 4.2" to 573°K and at several strain rates. Carbon was found to strengthen thorium primarily by increasing the thermally activated component of the flow stress. The strengthening due to carbon was directly proportional to the carbon content and decreased rapidly with increasing temperature up to 423" K. The flow stress also increased with increasing strain rate. The strengthening appears to be due to a strong short-range interaction between carbon atoms and dislocations. A yield point was observed in the Th-C alloys which increased with increasing carbon content. JTREVIOUS study of the mechanical properties of thorium has been confined largely to the measurement of the engineering properties. Work prior to 1956 has been summarized by Milko et al.1 who reported that additions of carbon to thorium sharply increased the room-temperature strength. In addition, the yield strength was observed to decrease rapidly over the temperature range from 25" to 500°C. In 1960, Klieven-eit2 measured the flow stress of thorium containing 400 ppm C. He found that over the temperature range from 78" to 470°K the flow stress was strongly dependent on temperature and rate of deformation. A drop in the load-elongation curve, or a yield point, was observed over most of the above temperature range. Above 470°K, the flow stress was nearly independent of temperature and strain rate. This strong temperature and strain rate dependence of flow stress is not generally observed in fcc metals. It is, in fact, more typical of the behavior reported for bcc metals. Bechtold,3 Wessel,4 and conrad5 have pointed out the striking difference between the commonly studied bcc metals and fcc metals in regard to the effect of temperature and strain rate on the flow stress. Zerwekh and scott6 studied the plastic deformation of thorium reported to contain 12 ppm C. They found that this material did not obey the Cottrell-Stokes law as expected for fcc metals. In addition, they found values of the activation volume smaller by an order of magnitude than expected for an fcc metal. They concluded that thorium was strengthened by a randomly dispersed solute. Thorium differs from many other fcc metals that have been studied extensively in that it shows a relatively high carbon solubility at room temperature. Mickleson and peterson7 report the solubility limit at room temperature to be 3500 ppm C. The lowest value reported is that of Smith and Honeycombe8 who report the limit to be 2000 ppm C at 350°C. The pres- ent investigation was a systematic study of the flow stress and yield point phenomenon of thorium over a broad range of carbon content, temperature, and strain rate. EXPERIMENTAL PROCEDURE The thorium used in this investigation was produced by the reduction of thorium tetrachloride with magnesium as described by Peterson et a1.' Chemical analysis of the original ingot after arc melting and electron beam melting is shown in Table I. Alloys were prepared by arc melting this thorium with high-purity spectrographic graphite. Threaded specimens with a gage length 0.252 in. diam by 1.6 in. long were used for the constant stress or creep measurements. These specimens were machined from rod which had been cold-rolled and swaged to % in. diam. Tensile specimens were prepared by swaging annealed 3/8 -in.-diam rod to 0.102 *0.001 in. The as-swaged wire was cut to lengths of 2 in., annealed, and the center 1-in. gage length elec-tropolished to 0.100 ±0.001 in. The specimens were gripped for a length of 3 in. at each end by a serrated four-jaw collet which was tightened by a tapered compression nut. No slipping occurred in the grips and negligible deformation was observed outside the 1-in. gage length. Both the creep and tensile specimens were annealed at 730°C under a vacuum of 1 x X Torr. The resulting structures consisted of equiaxed recrystallized grains with a grain size of 3200 grains per sq mm for the tensile specimens and 2200 grains per sq mm for the creep specimens. After the specimens were prepared, samples were analyzed for nitrogen, oxygen, and hydrogen. The results of these analyses are given in Table 11.

Jan 1, 1969

By John A. Hosking

The recent activity of numerous foreign mining companies in the once flourishing tin fields in Cornwall, England has resulted in renewed interest in the evaluation of hypothermal tin deposits. These deposits are mainly narrow tabular bodies and are usually steeply dipping. They exhibit thermal zoning the mineralization changing from lead/zinc through copper to tin with depth. The tin zone virtually never exceeds 1,000' in depth and the ore shoots within this zone tend to be erratic and localized. The grade which is presently considered to be economic is about 0.7% Sn. , this means a concentration of about l% cassiterite (the only economic mineral) which, being twice as heavy as the gange, represents only. 5% of the lode volumetrically. Within the lode, only one third may reach this economic grade and values within the shoots can range from 100% cassiterite to zero over a few inches. The enormity of the problem of evaluating such a deposit has not been fully appreciated by the companies involved whose experience has, for the main part, been in larger and more predictable ore bodies. This paper attempts to put these problems into perspective and out- lines the useful applicatations of statistical and computer techniques. It also stresses the need for enlightened interpretation of data by men familiar with the problem and that even in this day and age, educated, intuitive deduction should not yet be relegated to the limbo of alchemy and witchcraft.

Jan 1, 1969

By David L. Holt

It is well-established that hydrostatic pressure distribution is hardly achieved during uniaxial compaction of powders. All the previous investigations1-4 give consistent results and this variation is attributed to the die-wall friction. The conclusions are based on measurements of the density of very small portions of the compact. Although the analysis of the density or the strain distribution in the compact is very helpful in obtaining information about the stress distribution within a powder compact, it does not describe the problem from a more fundamental point of view. The densification in metal powder compacts takes place chiefly by plastic deformation (ignoring particle rearrangement) at the points of contact of the powder particles. The onset of yielding and subsequent growth of the contact areas (for spherical powders) take place fixed by a constant stress equal to three times the yield stress in tension or compression,5-7 assuming little or no work hardening. Therefore, by deforming spherical powders in the die and measuring the contact areas on each particle, the load at each contact point can be determined. In the present investigation, this was done by hot-pressing uniform spheres of lead, K-Monel, and sapphire. The details of the experiment have been described elsewhere.' The spheres were studied for the size and the number of contact points on each particle using a specially designed goniometer. It was found that the deformed faces that were approximately normal to the direction of pressing were about 2.2 times larger than those parallel to the direction of pressing. Fig. 1 shows the typical deformed sphere. A detailed study showed that the mean value of the contact areas on each sphere was within 5 pct for all the spheres in the die (ignoring those touching the die walls and the top and bottom of the die).' The spheres touching the die walls and the top and bottom of the die were found to have larger contact areas (8 to 10 pct) which indicates higher pressures in these regions of the compact and thus higher compact densities in these regions. These results show that density distribution calculated from such an experiment will give results consistent with the previous investigators. It is concluded, therefore, that the pressure distribution in the die is better understood by studying contact areas on each particle. 'R. Kamm, M. A. Steinberg, and J. Wulff: Trans. TMS-AIME, 1947, vol. 171, p. 439. 'Pol Duwez and Leo Zwell: I. Metals, 1949, vol. 1, p. 137. 'G. C. Kucynski and I. Zaplatynskyj: Trans. TMS-AIIME, 1956, vol. 206, p. 215. 'R. P. Seelig and J. Wulff: Trans. TMS-AIME, 1946, vol. 166, p. 492. 'H. Hencky: Z. Angew. Math. Mech., 1923, vol. 3, p. 241. "J. Ishlinsky: I. Appl. Math. Mech. USSR, 1944, vol. 8, p. 233. 'D. Tabor: Proc. Roy. Soc. (London), Ser. A, 1948, vol. 192, p. 247. 'Ashok K. Kakar and A. C. D. Chaklader: 1. Appl. Phys., 1967, vol. 38, p. 3223. Superplasticity in 60Zn-40Al David L. Holt THE occurrence of superplasticity in Al-Zn alloys is of interest because of its possible industrial exploitation.' The eutectoid composition (78Zn-22A1) has been the most extensively studied;'-= neck resistant flow and high strain rate sensitivity of flow stress (characteristic of superplasticity) are associated with a micron-size grain conferred on the alloy by an homo-genization and quench.5'6 Compositions away from the eutectoid have received comparatively little attention, especially from the viewpoint of relating the structural

Jan 1, 1969

By Lawrence Dykers

The paper presents a generalized history of the growth and utilization of electronic data processing in a medium- size, mining-oriented company. A brief narrative outlines a corporate wide data gathering system, its hardware and application. Responsibility areas for corporate accounting, operations control, engineering, and research program development are defined. A Synopsis of programs within responsibility areas is presented along with a review of program language requirements for each of these areas. Anticipated additional uses of computers and the programs being developed for these uses are outlined. The scope and growth of an Information Systems Department within Duval Corporation is briefly discussed. Suggestions are presented which should help minimize the problems and avoid some of the pitfalls of program development for those contemplating the initiation or revision of an electronic data processing system. The importance of lucid and comprehensive program documentation is stressed.

Jan 1, 1969

By R. W. Nelson

The theoretical basis is presented for energy dissipation methods of measuring permeability in saturated heterogeneous media. Analysis starts with the equation for single-phase flow in heterogeneous porous media which is a first-order partial differential equation in the unknown permeability. This equation is reduced to a system of characteristic equations useful in deriving a differential expression for the permeability as a function of the known potential distribution. For steady flow systems the expression is integrable, giving the permeability integral for direct calculation of the distribution along successive streamlines. The boundary condition in permeability is presented and includes a discussion of the special requirement to assure uniqueness. Theoretical results and necessary computations are incorporated into two general computer programs capable of determining the permeability distribution in two- and three-dimensional steady flow systems. Results are then presented for an energy dissipation analysis using the methods and soltware to determine a field permeability thickness distribution. INTRODUCTION Theoretical work leading to the description of fluid flow in heterogeneous porous media has developed slowly and somewhat sporadically, although the areas of engineering applications predominantly involve flow in nonhomogeneous media. The lack of accurate and economical methods for measuring field permeability distributions has been a major limitation to realistic description of natural flow systems. The economical measurement of permeability using energy dissipation methods may overcome this limitation. Among other things, any permeability measurement method involves consideration of energy dissipation; as used here, "energy dissipation method" denotes the following general approach. The areal energy distribution is measured on an existing flow system in porous media. Then through appropriate analysis of the dissipation of energy in the flow system, the permeability distribution is determined throughout the region using the minimum boundary conditions required to assure a mathematically unique result. This paper presents the theoretical basis for such a method, as well as the techniques and computer software needed to carry out the analysis. The method and techniques are then used in a preliminary field application. EQUATIONS DESCRIBING FLOW IN HETEROGENEOUS MEDLA Heterogeneous as used here implies differing in kind, having unlike quantities or possessing different characteristics. Accordingly, a heterogeneous porous medium has unlike quantities or differing characteristics at different locations. More precisely, if a porous medium is heterogeneous with respect to some property, then that property is functionally dependent on the spatial location. (Media properties are considered here as macroscopic.) Specifically considering permeability k,** then k = G(x, y, z) ,............(1) or the permeability is a scalar function G of the location (x, y, z). Spatial variation of several other properties, of which porosity, dispersivity and medium compressibility are but a few, is implied by the broad title of heterogeneous porous media. The term will be used hereafter to imply only heterogeneity with respect to permeability. The porous medium is considered isotropic as implied by G being only a scalar function. Anisotropy

Jan 1, 1969

By J. T. Clancey

The potential inadequacy of natural gas reserves to supply projected requirements in the 1980's has been pointed out.(1,2) As a result, interest has arisen in the development of new, potentially low-cost processes for the conversion of coal into high BTU gas. In June, 1964, the office of Coal Research (U. S. Department of interior) and Consolidation Coal Company (now a subsidiary of Continental Oil Company) entered into a contract to continue work on coal gasification utilizing the Consol CO2 Acceptor Process. Work under this contract has been specifically directed toward the use of lignite as the carbonaceous feed, although the process is also applicable to non-caking subbituminous coals. The primary objective of this work was to establish the technical feasibility in continuous bench-scale equipment, of the novel features of the C02 Acceptor Process. Secondary objectives were the testing of commercially obtainable acceptors and the design and economic evaluation of a commercial facility. The bench-scale process development has been completed successfully and the construction of a large pilot plant at Rapid City, South Dakota, has been authorized. It is the purpose of this paper to review the technology of this new gasification process and to present the current projected economics of a plant producing 250 MM SCFD of pipeline quality gas.

Jan 1, 1969

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 John C. Gifford, Charles L. Thomas

A unique and reproducible method is presented for the determination of water vapor in tough pitch wire bar copper. The procedure involves reduction of the water vapor with molten aluminum to form hydrogen, which is subsequently measured by mass spectroscopy. Average water vapor pressures within the porosities of the wire bar samples are calculated. Correlation is to exist between the specific gravities of the samples and their measured water vapor contents. The method should find application as a very sensitive means of detecting hydrogen embrittlement in copper. The nature and quantity of gases evolved and retained during the horizontal casting of tough pitch wire bar copper have long been of interest to the metallurgist. Considerable work has been done at this laboratory on the determination of these gases. The work has involved not only qualitative but also quantitative analysis, so as to provide a basis for a total accounting of the porosity which is associated with the cast product. From a knowledge of the gas-forming elements within the copper, and the practice of melting and protecting it with a reducing flame followed by contact with a charcoal cover in the casting ladle, the gases which one might expect to find in the pores of the cast product are sulfur dioxide, carbon monoxide, carbon dioxide, hydrogen, and water vapor. Hydrogen sulfide, nitrogen, and hydrocarbons would be other possibilities; however vacuum fusion-mass spectroscopy techniques employed at this laboratory have shown that no hydrogen sulfide and only traces of nitrogen and methane are present. It is highly improbable according to phillipsl that any sulfur dioxide could be evolved in wire bar copper with 10 ppm or less sulfur under normal freezing conditions. Mackay and smith2 have noted that porosity due to sulfur dioxide only becomes noticeable at concentrations above 20 ppm S. Investigation of carbon monoxide and carbon dioxide by a variation in the method of Bever and Floe showed that these two gases could only account, at 760 mm and 1064°C (Cu-Cua eutectic temperature), for a maximum of about 25 pct of the total porosity in a wire bar having a specific gravity of 8.40 g per cu cm. phillips' has noted that no normal furnace atmosphere is ever sufficiently rich in hydrogen to cause porosity in copper from hydrogen alone. In addition, using a hot vacuum extraction technique for hydrogen,4 values have never been observed in excess of 10 ppb in tough pitch wire bar. On the basis of the preceding considerations of gases in tough pitch wire bar, only water vapor is left to account for the major portion of the porosity. Direct determinations of water vapor are virtually impossible at low concentrations by any presently known technique, due to adsorption and desorption within the walls of the apparatus used.5 The present investigation deals with a method for the determination of water vapor by an indirect procedure, using molten aluminum as a reducing agent to form hydrogen according to the reaction: 2A1 + 3H2O — A12O3 + 3H2 The evolved hydrogen can then be measured quantitatively by mass spectroscopy. EXPERIMENTAL A 10-g piece of 99.9+ pct A1 was charged into a porous alumina crucible (Laboratory Equipment Co., No. 528-30). Fig. 1 shows the crucible in place at the bottom of an 8-in.-long quartz thimble. A funnel tube with two l1/8-in.-OD sidearms extending at a 90-deg angle from each other was attached to the top of the thimble. One of the sidearms was joined to the inlet system of the mass spectrometer (Consolidated Electrodynamics Corp. Model 21-620A) via a mercury diffusion pump situated between two dry-ice traps. The copper samples were placed in the other sidearm, followed by a glass-enclosed magnetic stirring bar for pushing the samples into the crucible. All ground joints were sealed with vacuum-grade wax. The entire system was evacuated and the aluminum was heated with a T-2.5 Lepel High Frequency Induction Furnace for 21/2 hr at a temperature visually estimated to be 900°C. The temperature was then lowered and the hydrogen was monitored on the mass spectrometer until it was given off at a constant rate of about 4 to 5 1 per hr. This rate corresponded to a slope of 2 to 3 divisions per min on the X3 attenuation of a 10-mv recorder at a hydrogen sensitivity of approximately 100 divisions per 1. A micromanometer (Consolidated Electrodynamics Corp. Model 23-105)

Jan 1, 1969

By D. E. Wolfson

This report presents 900° C BM-AGA carbonization and related data for coals from the principal beds of Nicholas, Randolph, and Webster Counties, W. Va. Thirty-three samples from nine coal beds in three counties were car-bonized at 900° C in the l8-inch-diameter BM-AGA retort, data from which have been correlated with industrial production. Host of the samples were chemically suitable for metallurgical use, and their coking properties were satisfactory. Except for four of the Lower Kit-tanning samples, the ranges of constituents in the coal seams were 1.8 to 9.0 percent ash and 0.4 to 1.1 percent sulfur, values within the range of accept-ability for metallurgical coals. Coke strength indexes were normal for Appalachian coals of similar rank, and the tumbler stability indexes of the coke ranged from 35 to 57.

Jan 1, 1969

The C.S.A. copper lead zinc mine, located seven miles north of Cobar in Central Western New South Wales, is the largest known mineral occurrence in the Cobar Mining Field. Hosted by the steeply west dipping, west facing sediments of the Cobar Group, the generally discordant orebodies occur within a strike width of 600 ft and an overall strike length of 1200 ft. They comprise lenticular steeply north pitching and east dipping zones of sulphide mineralisation which range in composition from massive pyrite-sphalerite-pyrrhotite--galena to less massive pyrite- pyrrhotite-chalcopyrite varieties. The thinly bedded siltstones, shales and graywackes hosting the mineralisation appear to have derived many of their constituents from volcanic sourcesä They have been metamorphosed to the greenschist facies of regional metamorphism. At least two stages of deformation and folding have occurred. The first stage folded the rocks on a south pitching fold axis into their present configuration, and super- imposed a strong axial plane cleavage which subsequently guided the emplacement of the mineralisation. The second stage of deformation is considered to have controlled the zonal distrib- ution of the orebodies and the appropriate fold axis appears to coincide with the long axis of the orebodies.

Jan 1, 1969

By B. Wilshire, W. J. Evans

The high-temperature creep properties of nickel, zinc, and iron have been determined over a range of stresses. The creep strain, E, was found to vary with time, t, as: where e0 is the instantaneous strain on loading, ET the total transient creep strain, $ the steady creep rate, and m is a constant relating to the rate of exhaustion of transient creep. Deviations from this relationship occurred during the initial 10 to 15 pct of the transient stage. These deviations result in the initial creep rate, go, calculated as (m . ET + es), being considerably lower than those obtained by measurements on the creep curve. For all materials, the initial creep rate, the constant m, and the duration of transient creep are all related to the steady creep rate. These relationships suggest that transient and steady-state creep should not be regarded as distinct stages.

Jan 1, 1969

By R. L. Rough

The Bureau of Mines analyzed rotary-coring-operations data to compare mud and air as coring mediums, and to compare core recoveries, penetration rates, and cost data for the respective mediums as part of an investigation of the susceptibility to secondary-recovery techniques of petroleum reservoirs in Ohio, Pennsylvania, and West Virginia. This report describes the rotary-diamond coring equipment and operations employed while coring 20 wells--10 cored using mud, and 10 cored using air. Data relevant to the draw works, rotary-table power, drill pipe, drill collars, core barrel, core head, mud pumps, or air compressors are tabulated. Average bit weight and rotary speed, core recovery, and penetration rates are listed for each formation cored. In general, core recoveries were better from the mud-cored wells, whereas penetration rates were faster for the air-cored wells. Coring costs were about the same for single-formation wells cored with either mud or air; however, costs increased considerably when multiple-formation wells were cored with air.

Jan 1, 1969

By R. G. Garlick, M. Garfinkle

It was observed for several bcc metal crystals that the Knoop hardness anisotropy was dependent essentially on the direction of the lung axis of the indentor alone and not on the plane of indentation. The generality of this observation was tested for an fcc md an hcp metal and an ionic crystal. For cubic crystals, this observation was valid; for the hcp structure, however, the planes of indentation did have an effect on the hardness anisotropy, although this was not nearly as significant as the direction of indentation. Because the direction of indentation is the only significant crystal-lographic parameter necessary to describe the hardness anisotropy, it is possible to represent the anisotropy of single crystals on the standard stereographic triangle. THE commonly observed1, 2 periodic variation of indentation hardness with crystallographic direction on the high-symmetry planes of various single crystals has been inadequately related to the physical or mechanical properties of the crystals examined. In fact, the hardness anisotropy curves for the various planes of a particular metal crystal, as is illustrated in Fig. 1, are uncorrelated and appear in the literature3, 4 as unrelated observations. Attempts to correlate hardness anisotropy curves with specific physical properties can be generally divided into either mechanistic or nonmechanistic approaches. A nonmechanistic approach would be to devise a mathematical expression that could describe the various hardness anisotropy curves. Such a relation could then be compared with the known anisotropy of various physical properties to determine which contribute to the observed hardness anisotropy. No such mathematical expression has been found in the literature.

Jan 1, 1969

By A. E. Dwight, A. F. Berndt

ThE published U-Ru equilibrium diagram indicates the existence of six intermetallic compounds in this system.' The structure of only two of the compounds, u2Ru2,3 and URU3,4 have been identified. This communication reports on the crystal structure and density of Uau3, which is formed by a peritectoid transformation at 1025° ± 5°C: U3Ru4 + U3Ru5 = U2Ru3. An alloy with the stoichiometric formula U2Ru3 was prepared by arc melting electrolytic uranium and ruthenium of 99.9 pct purity on a water-cooled copper hearth under an argon atmosphere. After homo-genization at 1000°C for 3 days, a metallographic examination revealed that the peritectoid transformation was complete and less than 5 pct of a second phase was present. A powdered sample, obtained by crushing the brittle compound, was annealed for 1 hr at 1000°C and air-cooled. Debye-Scherrer patterns were obtained with filtered CrKa, FeKa, CoKa, or CuKa radiation. The X-ray patterns of U2Ru3 weFe indexed as an fcc structure with a. = 12.895 0.00lA. The unit-cell constant and its standard deviation were calculated by a computer program described by Mueller, Heaton, and Miller.5 The density, measured by an immersion method, was 14.45 g cm-3. A calculated density of 14.48 g cm-3 was obtained on the assumption that twenty-four formula units (120 atoms) comprise a unit cell. The space group is either oh7 Fd3m, or the less symmetric, T4h, Fd3, since reflections indexed as hk0 with h + k + 4n are absent. All values of h2 + k2 + 12 permitted by both space groups are listed in Table I together with dc, do, and I. values. The calculated d spacings were obtained by the computer program of Mueller, Meyer, and simonsen.6 The observed d spacings above 0.77A were obtained from X-ray" patterns prepared with CuKa radiation, above 0.90A with CoKa radiaaion, above 0.98A with FeKa radiation, and above 1.16A with CrKa radiation. An attempt was made to identify the crystal structure of U2Ru3 by comparison with published data on other A2B3 compounds. A recent compilation7 of intermetallic compounds lists thirty-two structure types with the A2B3 stoichiometry. Only two of the structure types are fcc and they are Sb2O3(r), senarmontite, with 16 Sb2O3 per unit cell, and In2Te3 for which several structures have been proposed.8 However, the two cases cited do not have twenty-four formula units in the unit cell. We therefore, cannot identify UPRU3 with any of the other known A2B3 compounds. Ternary alloys were made in which 5 at. pct Os, Rh, or A1 were substituted for 5 pct of the Ru in U2Ru3. The osmium substitution increased the unit cell constant to 12.899 * .001A, which is to be expected since the atomic volume of osmium is slightly larger than

Jan 1, 1969

By B. J. Dalton

The Bureau of Mines Helium Research Center has as a long-range objective the development of an equation of state for helium that will allow all of the thermodynamic properties to be calculated within the accuracy with which they are known. If this objective is to be realized, a method of calculation must be known. This report gives the principles of the method we use in such problems. A computer program was developed for predicting these properties, including those at the critical point, that is perfectly general and applicable to any equation of state. To demonstrate the efficacy of our method, this computer program was used to evaluate thermodynamic properties of a Redlich-Kwong fluid in the two-phase region. Expressions for calculating various thermodynamic functions specific for this particular equation of state are derived. Numerical values are tabulated and graphs are presented for all functions calculated. It is shown that for a Redlich-Kwong fluid there are finite discontinuities in (1) the second temperature derivative of the Gibbs free energy or chemical potential at the critical point, (2) the second derivative of the vapor pressure curve with regard to the temperature on passing through the critical point, and (3) the measured heat capacity at constant volume on passing through the critical temperature when the calorimeter is filled to the critical density. It is also shown that the heat of vaporization is infinite for a Redlich-Kwong fluid at absolute zero.

Jan 1, 1969