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By T. Egleston

At the Dover meeting of the Institute, Mr. F. A. Canfield showed some of the members a machine which he had invented for dressing mineralogical and geological specimens, which he has since modified and brought to such a high state of perfection, that after having used it for several months in preparing specimens for the cabinet of the

By Lyden, Joseph P.

THE Picher Mining Field, fig. 1, which lies between Baxter Springs, Kansas, and Commerce, Okla., is the most intensely mineralized and the largest zinc-lead ore producing area in the Tri-State District of Missouri, Kansas, and Oklahoma. It has a vast lateral extent of underground workings that is unequaled for the observation of the geology of zinc-lead ore bodies in sedimentary horizons; and thousands of churn drill holes in the unmined areas supplement the underground observations with useful data for the interpretation of the geology. This paper is confined to the ore deposits of the Picher mining field. The reader is referred to the bibliography for the general geology of the Tri-State district which has been ably covered by many geologists. The writer was co-author of several publications on the Tri-State district.- This paper is necessarily a repetition of parts of those publications but contains a few changes and additions on the deposition of the minerals. The parts of this paper concerning mineralization maps and pipe slump-structures are not covered in the above publications.

Jan 1, 1950

By R. V. Smith, E. J. Dewees, R. H. Williams

Before this paper was presented, the terms "f" and "v1/f in flow equations had been called "friction coefficient" and "friction factor," respectively. However, many authors have used the names for the terms interchangeably, with the result that considerable confusion has existed in the literature on flow of fluids. In an effort to establish a clear and concise terminology for these terms, the authors have designated f as "resistance coefficient" and dm as "transmission factor." Transmission factors for the flow strings of gas wells were determined by tests on wells in six fields of Oklahoma, Texas, and Louisiana. Data were collected on 14 gas wells while gas was flowing through 1 1/4, 2, 21/2, and 3-in. tubing and 51/2 and 7-in. casing. The transmission factors developed from these data were found to follow the resistance equation published by Nikuradse1 for turbulent flow in "rough" pipes with an average absolute roughness of 0.000,65 in. This average absolute roughness is believed to be representative generally of the flow strings of gas wells with the exception of those that have been exposed to corrosion or other conditions causing undue roughness. Also, use of an absolute roughness of 0.000,65 in. probably will result in transmission factors that are more representative of gas-well conditions than those in common use today, provided that the transmission factors are calculated by the methods outlined in this report. The authors believe that use of these transmission factors will permit calculation of more accurate subsurface pressures in gas wells than those in use today. Engineers use transmission factors in flow equations to compute subsurface pressures in flowing gas wells from measured wellhead pressures. These subsurface pressures are necessary for determining the productivity of gas wells from "back-pressure" tests. The methods of calculating pressures in flowing gas wells, as outlined by Rawlins and Schellhardt2 in Bureau of Mines Monograph 7, are based on the transmission factors in the well-known Weymouth formula" Natural gas engineers have realized that errors introduced by using transmission factors as given by the Weymouth formula are relatively unimportant in testing low-capacity gas wells; but they also know that such factors are important considerations in testing large-capacity wells. Accordingly, the research described in this report was undertaken to fulfill the need for more accurate means of calculating subsurface pressures in gas wells. This report is part of the Bureau's study of the flow of natural gas through pipe and commercial pipelines. Several of the conclusions regarding flow in the flow strings of gas wells were influenced by the results of the study of flow in horizontal pipelines. These instances are mentioned in the text of this report. METHODS OF COMPUTING TRANSMISSION FACTORS Methods and procedures for computing transmission factors for turbulent flow in circular pipes from test data taken on gas wells have been derived and explained in detail in a paper by Smith4. As these methods were used to calculate the transmission factors presented in this report, a summary is included. Starting with

Jan 1, 1955

By Arnulf Muan, Klaus Schwerdtfeger, L. S. Darken

The equilibrium ratios CO/CO, of. a gas pharse coexislitrg with selected oxide phase assemblages of the system "FeO"-MnO-SiO2 and metallic iron have been determined at 1150°C. The data obtained are combined wilh the thermodynamic data on fayalite (Fe2SiOi) and "FeO"-MnO solid solutions to derive the actiuity-coiHpQsiUon relations for the various oxide components of the olivine (Fe2SiO4-,lIn2Si04) and pyroxenoid (standard free energies of formation of ferrosilile (FeSiO,), tephroite , and rhodonite from their oxides have been evaluated. In the Appendicc~s by Darken and Schivcerdtjeger the ideal solution law for solid deri oed. THE quaternary system Fe-Mn-Si-0 is of interest in many important phases of iron- and steelmaking. For instance, reduction in the blast furnace of ores containing Fe-Mn silicates, deoxidation of liquid steel with Mn-Si alloys, formation and subsequent alterations of oxide inclusions in steels, and the oxidation of manganese- and silicon-containing steels during processing are all governed largely by the thermodynamic relations existing in the system Fe-Mn-Si-O. Although the equilibria between liquid iron and Fe-Mn silicates have been studied in detail previously,' experimental data are lacking for equilibria among the solid phases. The present paper provides such data for a selected temperature, 1150°C. I) PREVIOUS WORK The general feature of subsolidus phase relations in the system iron oxide-manganese oxide-silica under strongly reducing conditions is known.' Fig. 1 represents an isothermal section at 1150°C. The phases present, in addition to silica, are three solid-solution series, viz.. the oxide solid-solution series "Fe0"-MnO (manganowiistite), the orthosilicate solid-solution series Fe2SiO4-Mn2SiO4 (olivine), and the metasilicate solid-solution series FeSi03-MnSi03 (pyroxenoid). The "FeO"-MnO solid solution is continuous between the two end members wustite and manganositeV3 as is the orthosilicate series between the two end members Fe2SiO4 and Mn2 SiO4. 4 The metasilicate solid solution, on the other hand, extends only part way from the MnSi0.l end member toward FeSiO because the latter end member is unstable relative to the phase assemblage fayalite + silica. The letters a through m in Fig. 1 identify end members of the individual solid phases dealt with [for instance, c designates fayalite (FeZSiO4) in equilibrium with wustite, e designates fayalite in equilibrium with silica, and so forth]. In addition to the phase relations there are some thermodynamic data available for the end members of the silicate solid solutions and for the "FeO" -MnO solid solution. The free energy of formation of fayalite (Fe2Si04) from its oxide components has been studied by several investigators. Unfortunately, the data obtained show considerable discrepancies. According to recent tabulations by Kelley, the change in standard free energy Affn for the reaction

Jan 1, 1967

By Nicholas J. Grant, David S. Bloom

An investigation of the Cr-Ni system has revealed that there exists a eutectoid transformation at about 1180°C. 'The transformation in chromium implied by the eutectoid reaction was detected at about 100°C below its melting point. Associated with the eutectoid transformation, a metastable transition structure has been found. THE Cr-Ni phase diagram is shown in current literature to be a simple eutectic system in which the high chromium end of the diagram is incompletely determined, Fig. 1. The last investigation of this system was undertaken in 1936.' Because of limitations in metal purity, especially of chromium, and temperature measuring techniques, the diagram should be accepted with some reservations, as was indicated by Hansen.V or examwle.-, the wresence of the compound Cr²Ni, with a tetragonal structure," remains unverified and incompatible with the simple eutectic diagram. The work reported here began because of discrepancies that appeared in experimental studies in the binary alloys Cr-Ni and in the ternary system Cr-Mo-Ni. The existing binary Cr-Ni diagram failed to provide a complete explanation of observations made by microscope, X-ray, and thermal analyses. Experimental Methods The materials employed were of a higher degree of purity than were available to previous investigators. The Mond nickel used had a nominal purity of 99.87 pct, while the electrolytic chromium analyzed 99.03 pct with the major impurity being 0.5 to 0.7 pct oxygen with some iron. All alloys were melted in a vacuum furnace to remove dissolved gases, sufficient carbon was added to the charge to combine with all the oxygen as CO. Final analysis determined the carbon as about 0.02 pct and the oxygen around 0.06 pct or slightly more. Stabilized zirconia crucibles and thermocouple protection tips were used throughout and contributed no detectable impurity to the melts, as long as the oxygen in the chromium was kept low. Heats averaged about 250 g, which permitted about 2 in. of the thermocouple protection tips to be submerged. The temperature drop across the thermocouple protection tip was determined to be about 3°C, a minor source of error. The alloys, after removal from the vacuum furnace, were placed in a furnace operating in a purified argon atmosphere for the thermal analyses. An- nealed wolfram-molybdenum thermocouples provided the primary means of temperature determination, though a Pt-Pt-10 pct Rh couple was employed for a check when possible. A sensitive, high-speed Leeds and Northrup Speedomax recording potentiometer indicated the thermocouple output. X-ray diffraction patterns were obtained primarily on a Norelco unit, which permitted diffraction angles only up to 45" (28 = 90"). In general, either rotated or stationary solid samples were used, because it later evolved that many samples were susceptible to transformation resulting from the cold working involved in pulverizing. It was also noted that rotating a sample sometimes suppressed weak lines, so, usually, samples were not rotated. Later a high temperature camera was adapted for use at temperatures up to 1400 °C on the Norelco unit utilizing both solid and powdered samples. Unless otherwise noted, all X-ray patterns were made with a chromium tube and a vanadium filter. Further-

Jan 1, 1952

By John T. Norton, Matthew J. Donachie

Residual lattice strai?zs were produced in 2024 aluminum and ingot iron by uniaxial tensile deformation. These strains were rneasured on the original surface and ulith depth below the surface. The strains conformed approximately to those from a macroscopic stress distribution but they were not truly macroscopic in nature. The exact mechanism which apparently causes the coherently difi9,acting region of each grain to behave as if macroscopically stressed was not determined. MACROSCOPIC stresses in metals produce strains in the lattice which result in X-ray line broadening and line displacements. The latter effect can be utilized in a technique for determining stresses in metals as first shown by Lester and born.' Subsequent advances in technique have enabled the X-ray method of stress measurement to be satisfactorily applied to many problems involving residual stresses of a macroscopic nature, such as those due to welding, grinding, shot-peening, and so forth. In the case of stresses such as those described above, the correlation of X-ray- and mechanically determined data has been generally good. However, plastically extended polycrystalline metals have sometimes been reported2 to show line displacements upon release of the applied tensile load, yet the nature or origin of the residual lattice strains, rls, producing these displacements has never been clear. As will be pointed out, this lack of clarity regarding the macroscopic or microscopic nature and origin of these stresses casts doubt on the validity of results achieved by the commonly accepted techniques of X-ray stress measurement. This anomalous behavior requires clarification to remove the doubts concerning X-ray stress measurement. The present paper is the result of an investigation of the interesting behavior of such plastically extended polycrystalline metal bodies. The studies were originated to carry out the following tasks: 1) Observe whether a residual lattice strain is produced as a result of plastic extension and show whether any residual lattice strains produced can be related to the usual concept of a macrostress. 2) Examine the origin of any residual lattice strains observed. 3) Consider the implications or consequences of the existence of such residual lattice strains on the problem of X-ray stress measurement. THEORY 1) Lattice Strains. The theoretical developments necessary for the treatment of lattice strains and their relation to stresses follow from the classical theory of elasticity and have been adequately covered by arrett. For an isotropic solid under homogeneous deformation, it can be shown that, for uniaxial stresses where Dl is the macrostress acting in the longitudinal direction; E$L is the lattice strain in the plane defined by the surface normal and the longitudinal direction at an angle, , from the surface normal; ET is the similar strain in the transverse plane; E is Young's modulus; and v is Poisson's ratio. Eq. [2] is independent of angle + and Eq. [I] is a linear function of sin2, see Fig. 1, and can be solved analytically for DL if E and u are known and EL is measured. Thus, a uniaxial macrostress will be indicated by a linear E,L vs sinZ plot and a

Jan 1, 1962

By J. S. Billheimer, B. H. Sage, W. N. Lacey, C. G. Yundt

As a part of a general investigation of the separation of bitumen from hydrocarbon mixtures a study was made of a restricted quaternary system composed of methane, decane, tetralin, and bitumen. The work was limited to a pressure of 8000 psi, a temperature of 220 °F, and to a fixed relative proportion of decane, tetralin, and bitumen. The measurements permitted the determination of the distribution of these components in each of the fluid phases. It was not possible to distinguish a second liquid phase in the course of these measurements. Gas-liquid equilibrium "constants" of each of the components were found to vary markedly with the composition of the system while temperature and pressure remained fixed. INTRODUCTION The separation of bitumen frorn naturally occurring hydrocarbon mixtures has been of importance for a number of years in the production of petroleum, especially in the California area. The deposition of this material from crude oils was noted in earlier studies of the solubility of natural gas in crude oil.¹,²,3 Studies of the separation of bitumen from crude oils from the Greeley and Santa Fe Springs fields were carried out."." The behavior of these systems appeared complex and studies of two restricted ternary systems involving mixtures of n-pentane, tetralin, and bitumen,' and of decane, tetralin; and hitumen, confirmed this belief. Reviews of the literature pertaining to the separation of bitumen from naturally occuring and refined hydrocarbons are available." The important effect of methane in the separation of bitu- men from naturally occurring hydrocarbon mixtures was apparent from the earlier studies and for that reason it appeared desirable to investigate a restricted quarternary system involving mixtures of methane. decane, tetralin, and bitumen; data concerning the behavior of mixtures of decane. tetralin. and bitumen having already been obtained.V his study was restricted to a pressure of 8000 psi," a temperatue of 220° F, and fixed relative proportions of bitumen, decane. and tetralin. This composite constituent, hereinafter designated as the less volatile constituent, was made up of 0.0455 weight fraction bitumen. 0.0909 weight fraction decane, and 0.8636 weight fraction tetralin. The experimental method involved bringing together mixtures of methane and the less volatile constituent in varying proportions in a constant volume container at the pressure and temperature indicated above. The composition of each of the phases was determined and from this the extent of the separation of bitumen was established. MATERIALS The bitumen used in this investigation was obtained from the same stocks employed in earlier studies. The crude material from the North Coles Levee field was stored in the laboratory] in a closed drum for a period of five years. Several samples from this stock were subjected to refining operations which were described earlier,' and every effort was made to follow the same procedure in all cases. It was necessary to prepare supplies of bitumen for this investigation at two rather widely different times. These materials have been identified as samples 1 and 2. The composition of the crude bitumen after it was washed with n-pentane at room temperature

Jan 1, 1949

By Rex E. Cheek, Donald E. Menzie

The fluid mapper, a model relatively new to the petroleum industry, was used to study the effect of various mobility ratios on the areal sweepout efficiency for two typical spacing patterns. The experiments indicated the areal sweepout for the five-spot pattern varied from 51.8 per cent at a mobility ratio of 0.093 to 89.1 per cent for a ratio of 24.4. In the direct line-drive pattern, the areal sweepout varied from 58.7 per cent at a mobility ratio of 0.089 to 92.0 per cent at a ratio of 24.8. The fluid mapper may prove useful to determine quickly the effective areal sweepout for any well spacing. INTRODUCTION The effect of the mobility ratio on the areal sweepout efficiency during primary depletion of a water drive reservoir and during secondary recovery operations has recently become more widely recognized The mobility ratio, M, is defined as: _ kjp (displaced fluid) k/u (displacing fluid) where k = effective permeability u = viscosity When the displacing fluid is miscible with the displaced fluid, the permeabilities are equal and the mobility ratio may be expressed as a ratio of viscosities: u (displacing fluid) u (displaced fluid) The mathematical analysis for calculating the areal sweepout efficiency with mobility ratio other than unity is quite tedious.5,11 An experimental method by using a potentiometric model2 in a step-wise manner and in using an X-ray shadowgraph model3,12 with continuous fluid flow has been published. Several types of models have been used to study oil and gas reservoir performance. These models may be classified as physical, electrolytic, potentiometric, X-ray shadowgraph, and fluid mapper. The X-ray shadowgraph and fluid mapper are models relatively new to petroleum engineering and have not been used extensively for specific applications. The theory of the fluid mapper indicates it may be adapted to a study of areal sweepout efficiencies for various mobility ratios as well as other complex problems in petroleum engineering. The use of the model and results obtained when using displacing and displaced fluids of equal densities but different viscosities are discussed. FLUID MAPPER DEVELOPMENT H. S. Hele-ShawV eveloped a fluid mapper model based on the hydrodynamic theory. This theory is that in the steady flow of a viscous fluid between horizontal parallel plates spaced a very small distance apart, the effect of viscous shear is of such magnitude in the vertical plane that the motion in the horizontal plane is practically undisbrted streamline flow. Techniques developed by Hele-Shaw were not expanded and no additional developments in fluid mapper models were forthcoming until A. D. Moore, University of Michigan, published a series of papers starting in 1949, which describe the construction of a flexible and inexpensive model'h nd the fluid mapper technique for the solution of certain problems.' The essential components of the fluid mapper as developed by Moore are::.ln 1. A base slab. made of dental stone (calcium sulphate and water). which is shaped to represent the prototype. 2. Plate glass slightly larger than the slab and spaced

Jan 1, 1956

By W. N. Lacey, C. G. Yundt, B. H. Sage, J. S. Billheimer

As a part of a general investigation of the separation of bitumen from hydrocarbon mixtures a study was made of a restricted quaternary system composed of methane, decane, tetralin, and bitumen. The work was limited to a pressure of 8000 psi, a temperature of 220 °F, and to a fixed relative proportion of decane, tetralin, and bitumen. The measurements permitted the determination of the distribution of these components in each of the fluid phases. It was not possible to distinguish a second liquid phase in the course of these measurements. Gas-liquid equilibrium "constants" of each of the components were found to vary markedly with the composition of the system while temperature and pressure remained fixed. INTRODUCTION The separation of bitumen frorn naturally occurring hydrocarbon mixtures has been of importance for a number of years in the production of petroleum, especially in the California area. The deposition of this material from crude oils was noted in earlier studies of the solubility of natural gas in crude oil.¹,²,3 Studies of the separation of bitumen from crude oils from the Greeley and Santa Fe Springs fields were carried out."." The behavior of these systems appeared complex and studies of two restricted ternary systems involving mixtures of n-pentane, tetralin, and bitumen,' and of decane, tetralin; and hitumen, confirmed this belief. Reviews of the literature pertaining to the separation of bitumen from naturally occuring and refined hydrocarbons are available." The important effect of methane in the separation of bitu- men from naturally occurring hydrocarbon mixtures was apparent from the earlier studies and for that reason it appeared desirable to investigate a restricted quarternary system involving mixtures of methane. decane, tetralin, and bitumen; data concerning the behavior of mixtures of decane. tetralin. and bitumen having already been obtained.V his study was restricted to a pressure of 8000 psi," a temperatue of 220° F, and fixed relative proportions of bitumen, decane. and tetralin. This composite constituent, hereinafter designated as the less volatile constituent, was made up of 0.0455 weight fraction bitumen. 0.0909 weight fraction decane, and 0.8636 weight fraction tetralin. The experimental method involved bringing together mixtures of methane and the less volatile constituent in varying proportions in a constant volume container at the pressure and temperature indicated above. The composition of each of the phases was determined and from this the extent of the separation of bitumen was established. MATERIALS The bitumen used in this investigation was obtained from the same stocks employed in earlier studies. The crude material from the North Coles Levee field was stored in the laboratory] in a closed drum for a period of five years. Several samples from this stock were subjected to refining operations which were described earlier,' and every effort was made to follow the same procedure in all cases. It was necessary to prepare supplies of bitumen for this investigation at two rather widely different times. These materials have been identified as samples 1 and 2. The composition of the crude bitumen after it was washed with n-pentane at room temperature

Jan 1, 1949

By B. L. Averbach, Morris Cohen, L. L. Seigle

Free energies, enthalpies, and entropies of mixing of Ni-Au solid solutions containing 5 to 95 atomic pct Ni have been determined by the electromotive force method at 700° to 900°C. The thermodynamic activities exhibit large positive deviations from Raoult's law, and the entropies of mixing are almost twice those of ideal solutions. The enthalpies of mixing are positive (heat is absorbed) and are attributable to the lattice distortional energy resulting from the size difference between the nickel and gold atoms. This factor appears to be responsible for the miscibility gap at lower temperatures. IN the thermodynamic study of metallic solid solutions, most interest has been directed toward systems with negative deviation from Raoult's law, namely, those exhibiting superlattice or compound formation. The results of previous investigations are summarized in recent publications.'-' Relatively little experimental work has been carried out on solid solutions which manifest a positive deviation, possibly because the range of solubility in such cases is usually quite limited. Nevertheless, the relationship of the thermodynamic properties of these solutions to diffusion, nucleation, and precipitation in the solid state are of considerable importance. The binary Ni-Au alloys are particularly suited to an investigation of these relationships. Despite the presence of a miscibility gap at lower temperatures, Fig. 1, indicating a large positive deviation from Raoult's law, complete solid solubility is found above 840°C. Moreover, the difference in the atomic scattering powers of nickel and gold is sufficiently great to permit X-ray diffraction studies of atomic arrangements and pre-precipitation phenomena. Radioisotopes of both nickel and gold are available for diffusion work, and finally, a large difference in nobility between the two elements facilitates measurement of the thermodynamic properties. The present paper describes the experimental determination of the free energies, enthalpies, and entropies of mixing of solid Ni-Au alloys. Table I gives a list of the symbols used in the paper. Experimental Method The stability of nickel chloride relative to gold chloride" indicated that the galvanic cell method could be used for determining the thermodynamic properties of Ni-Au alloys. An electrolytic cell (Fig. 2) was constructed, similar to that of Weibke and Matthes,7 in which the electrodes were solid nickel and Ni-Au alloys, and the electrolyte was a fused mixture of alkali chlorides containing NiCl,. The cell electrodes were made from fine gold granules and carbonyl nickel shot melted together under argon, chill cast, swaged to 1/16 in. diam rod, and annealed for one week at 850°C. Commercial reagent and chemically pure grade salts, purified by dehydration, were used for the electrolyte. The cell, operating in an atmosphere of purified argon, was heated in a resistance-wound cylindrical furnace whose temperature was controlled to within ±0.5ºC. The potential developed between the pure nickel and the alloy electrodes, which is related to the thermodynamic properties of the alloys by standard equations to be presented later, was measured with a potentiometer and a mirror galvanometer sensitive to 10-7 v. Dehydration of the electrolyte was carried out in the assembled cell by evacuating at 100°C for about

Jan 1, 1953

By P. Hudock

Thin films of PbS and CdS have been deposited on insulutiug- sapphire substrates by euzploying a subliwzation technique rising near-equilibriurum conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have mobilities approachitzg values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. By performing the depositiotz of a compound within a small chamber heated to a UNiform temperature within a Vacuum systerrz, it is possible to approach equiilibrium cod-tions r.~litl~irs the chamber. In this way; the sublimation and condensation proceed under near equilibrium co?zditions, and it was found that the properties of dePosited corrzpounds were similar to those of the source material. Oriented PbS films on sapphire have a roor?l- temperature unobility of 700 sq cm per v sec and a T-5/2 temperature dependence characteristic of bulk crrystnls. CdS layers on sapphive Izazse a resistivity ~uhich is corrlpamble to the resistivity of the souvce crystals over a range of four ordem of rrlagnitude. Irz contrast, Ihe resistivity of CdS films prepared by conventional evaporation depends largely upon the substrate terrzperat~ire and postheating treatrrletlt, vather than upon the properties of' the solirce rrraterial. In the case oj the CdS films the achievment of high carrier mobility required the cargful exclusion of cont~~~~ii~unts from the films. The steps taken to accomplish this included presublimation of the source material, performance of the deposition at a backg-m~ozd pressure less than 10-8 Torr, and a solvent extraction with liquid cadminum, similar to that described by Aven and woodbury. The deposition of ,films under near-equilibrium conditions is being op-plied to other classes oj COmpounds. II should he of 1:allce ,tor llle deposition of nny matevial that decomposes in the vapor state. THIN films of PbS and CdS have been deposited on insulating sapphire substrates by employing a sublimation technique using near-equilibrium conditions in ultrahigh vacuum. Oriented polycrystalline PbS and CdS films on sapphire have Hall mobilities approaching values characteristic of bulk crystals. In the case of CdS, special purification procedures were crucial in obtaining high-mobility films. Depositions were performed in a small quartz sublimation cell shown in Fig. 1 that contained the compound and the single-crystal sapphire substrate. The substrates were etched in tapered solutions of hot phosphoric acid, rinsed in deionized water, dried, and transferred to the cell under dry nitrogen. Graphite crucibles and substrates were used in experiments where it was necessary to provide an inert test vehicle for the analytical determination of impurities in the source crystals and deposited films. The crucibles and substrates were machined out of spectrographic-grade graphite having less than 1 ppm of impurities. A quartz mask was sometimes used to define a pattern which could be used for Hall and resistivity measurements. Close spacing between the compound and substrate was maintained to insure better transport of each component from the source material.

Jan 1, 1968

By AIME AIME

ON JULY 12, 1921, S. S. Arentz, representative at large from Nevada, introduced in the House of Representatives, under the number H. R. 7736, a bill to revise, amend and codify laws of the United States relating to the location of mining claims on public domain, and other purposes. This bill had been drafted by a committee of consulting engineers of the U. S. Bureau of Mines. The immediate purpose of this introduction in Congress was to make it avail- able for general information and discussion. In pursuance of this purpose Mr. Arentz issued the following circular: This proposed codification and revision of the mining laws of the United States as received from a committee of mining and metallurgical engineers appointed by the Director of the United States Bureau of Mines was introduced in the House of Representatives by the undersigned (who has operated and developed mines throughout the West for many years). It is submitted to prospectors, mine operators and mining engineers, all of whom are affected and vitally interested in the subject with the hope that they will give this bill their careful consideration and study.

Jan 1, 1921

MORE than 5000 miners and suppliers descended upon Denver to make the American Mining Congress' four-day metal mining show one of the most extravagant equipment displays ever assembled in one place at one time. The most recent developments in equipment for mining, milling, and processing ore were shown by the 146 exhibitors at Denver's new City Auditorium which covers 57,000 sq ft of floor space. Other displays were placed in the open air opposite the auditorium site. Registration desks were opened Sunday, Sept. 21. A field trip to the Colorado School of Mines at Golden was the featured activity of the day. Official opening of the show took place on Monday, and presided over by Howard I. Young, president of American Zinc, Lead & Smelting Co.; Otto Herres, vice president, Combined Metals Reduction Co.; William J. Coulter, vice president, Climax Molybdenum Co.; Charles B. Stainback, Westinghouse Electric Corp.; and Merrill E. Shoup, president, Golden Cycle Corp. Convention welcoming addresses were delivered by a representative of Mayor James Q. Newton, of Denver, and Gov. Daniel V. Thorton of Colorado. Following the formal opening ceremonies a round table discussion dealt with the "Paley Commission Report" formally called Resources for Freedom. Participating in the panel were: Arthur H. Bunker and George R. Brown, members of the Paley commission; H. I. Young, president of the American Mining Congress; Horace M. Albright, president of U. S. Potash Co.; Evan Just, vice president, Cyprus Mines Corp.; Donald H. McLaughlin, president, Homestake Mining Co.; E. H. Snyder, president Combined Metals Reduction Co.; Simon D. Strauss, vice president, American Smelting & Refining Co.; Sen. H. C. Dworshak (R.-Idaho) ; Ira B. Joralemon, consulting engineer; Jess Larson, De fense Materials Procurement Agency; and Andrew Fletcher, president of St. Joseph Lead Co. The panel discussed the report for six hours, adding a great deal of information to the already voluminous amount which has been gathered concerning it. Three objections to the report frequently mentioned were: 1-the multilateral contract; 2-international buffer stocks; 3-international buffer stocks combined with limited quota arrangements. Points on which the panel commended the report were its recommendations for acceleration of topographic and geologic mapping of the United States and Alaska; recognition of the principle of percentage depletion for metals and minerals; and advocation of removal of the present limitations on the expensing of exploration costs applicable to minerals. Technical sessions were held throughout the four days of the meeting. Included in the program were: Progress in Mechanication; Small Mines; Public Lands; Open Pit Mining; Manpower-Labor Relations; Shaft Sinking; Roof Support; Taxation, Gold, Silver and Monetary Policy; Advances in Mill Practices; Special Conference on Strategic Materials; Uranium Mining-Atomic Energy; Prospecting and Exploration; New Metallurgical Processes; and Rock Breaking. About 45 papers and several panels were presented during technical sessions. Formal and informal social functions consumed the remaining time of the convention. Three locations were needed to handle the huge throng attending the Mining Jamboree Monday evening. The only other sponsored social function took place Thursday evening. A great many informal gatherings, chiefly convivial, were held in manufacturers' courtesy rooms-called wet stopes. Field trips included Cripple Creek, Pueblo, Climax -Leadville-Gilman, Colorado Plateau-Grand

Jan 1, 1952

Sec. 1. This Division shall be known as the Institute of Metals Division of the American Institute of Mining and Metallurgical Engineers. Sec. 2. The object of the Division shall be to furnish a medium of cooperation between those interested in the metallurgy, fabrication and uses of the nonferrous metals and their alloys; to represent the A. I. M. E. in so far as nonferrous metallurgy is concerned, within the rights given in A. I. M. E. By-law XI., Sec. 1, and not inconsistent with the Constitution and By-laws of the A. I. M. E.; to hold meetings for social intercourse and the discussion of nonferrous metallurgy; to stimulate the writing, presentation and discussion of papers of high quality on nonferrous metallurgy; to reject or accept such papers for presentation before meetings of the Division. Article II—MembeRs Sec. 1. Any Member, Associate, or Junior Associate of the A. I. M. E. in good standing may become a Member, Associate or Junior Associate of this Division upon registering in writing a desire so to do, but without additional dues. Sec. 2. But no one who has been continuously indebted to the A. I. M. E. or to this Division for more than three months shall be entitled to vote or to receive publications to which, as a member of the Division, he would be entitled. Article III—Funds Sec. 1. The expenditure of the funds reccived by the Division shall be authorized by the Executive Committee of the Division. Article IV—Meetings Sec. 1. The Division shall meet at the same time and place as the annual meeting of the A. I. M. E., and at such other times and places as may be determined by the Executive Committee subject to the approval of the Board of Directors of the A. I. M. E. Sec. 2. The annual business meeting for election of officers shall be held within a few days before or after the annual business meeting of the A. I. M. E. Sec. 3. At any meeting of the Division for which notice has been sent to the members of the Division through the regular mail at least one month in advance, a business meeting may be convened by order of the Executive Committee, and any routine business transacted not inconsistent with these By-laws or with the Constitution or By-laws of the A. I. M. E. Sec. 4. For the transaction of business, the presence of a quorum of not less than 25 members of the Division shall be necessary. Article V—Officers and Government Sec. 1. The officers of the Division shall consist of a Chairman, two Vice-chairInen, Secretary and Treasurer. The office of Secretary and Treasurer may be combined in one person, if desired by the Executive Committee. Sec. 2. The government of the affairs of the Division shall rest in an Executive Committee, in so far as is consistent with the By-laws of the Division and the Constitution and By-laws of the A. I. M. E. Institute of Metals Divisiori

Jan 1, 1931

By W. M. Fox, D. P. Detwiler

IN the course of research on semiconducting inter-metallic compounds, it became necessary to obtain gallium metal of greater purity that that available commercially. Several methods were considered for further purification, including acid leaching,' fractional crystallization,' and zone-refining.3-5 The method of fractional crystallization was discarded as being equivalent to zone-refining in purification but inefficient in material and time. Both acid leaching and zone-refining were tried, and the method finally adopted is a combination of the two. The acid leaching technique has been reported' to produce gallium in which no impurities are detectable spectroscopically. Although this method is very effective in removing oxides and surface contaminants, semiconducting material made of gallium subjected only to leaching indicated little reduction in the concentration of metallic impurities. Zone-refining, however, appears very effective in removing trace metallic impurities, but comparatively ineffective in removing the surface oxide film. Consequently, the method evolved consists of acid leaching to thoroughly clean the surface, followed by zone-refining to remove metallic impurities. The low melting point and relatively high thermal conductivity of gallium introduce some difficulty in maintaining frozen and molten zones in zone-refining. To accomplish this, it is found necessary to reduce the effective ambient temperature by circulating ice water in coils about the regions that are to be kept frozen, while heat is supplied to the molten regions by resistance coils. The power supplied to the heating coils is regulated by a constant-voltage transformer and a variable autotransformer. Both heating and cooling coils are mounted on a transite base. The gallium ingot is held in a closed pyrex tube sliding inside the heating and cooling coils, the reciprocating method of Tanenbaum et al. being employed to move the molten zones through the ingot at a rate of 2 in. per hr. This apparatus is shown in Fig. 1. The results of a spectroscopic analysis f a zone-refined ingot, as well as of the material as-received and after acid leaching, are shown in Table I. The ingot was 32 cm in length, and received 37 molten-zone passes, the molten zone being about 4 cm long. The only impurity found was lead, the following elements being reported also as checked but not found in the pure material: Al, Sb, As, Ba, Be, Bi, B, Cd, Ca, Cr, Co, Cb, Cu, Ge, Au, Fe, Mg, Mn, Mo, Ni, Pt, Si, Ag, Na, Sr, Sn, Te, Ti, W, V, Zn, and Zr. There thus appears no indication of pickup of Al, Mg, or Si from the pyrex boat as reported by Zimmerman' in his fractional crystallization. Thus it appears that definite removal of lead from gallium occurs during the zone-refining process. It also may be concluded that a more sensitive analytical procedure than spectroscopy is required to evaluate quantitatively the purity of zone-refined metals. One such procedure which is proposed for use in the near future is the measurement of very low temperature resistivity. Although this will not identify the impurities present, it offers a very sensitive check of total impurity. Acknowledgment This work was supported by the Air Research and Development Command, United States Air Force.

Jan 1, 1956

By Regis M. N. Pelloux, N. J. Grant

Five or six alloys each in the systems Ni-C.v, Ni-Mo, and NL-W, spaced to cover the single phase areas as well as a part of the adjacent two-phase field, were prepared as uacuum-melted alloys. Tensile tests at room temperature and stress rupture tests at 1200° and 1500°F we.ve run for time periods to give fracture in 0.1 to 500 hr. Observations mere made of solid-solution and second-phase strengthening or uleakening, coupled with studies of ductility and the role of structure on the noted behavior patterns. THE development of stable creep-resistant alloys while broad and systematic is also highly empirical. A number of simple rules have been suggestedL-" but these are based on scant data. Whereas rules for low-temperature alloy strengthening can be applied with some success in more simple systems, the extension to behavior at high temperatures (greater than about 0.4 of the absolute melting temperature) is very poorly understood and has encountered important exceptions and deviations in terms of atom size or valency effects. In particular, the occurrence of both solid-solution weakening4,5 and second-phase weakening2 at high temperatures is of interest. MATERIALS AND PROCEDURE Nickel was chosen as the base material because of its important role in current high-temperature alloy applications, because of its freedom from a phase transformation, and because of wide solubilities for many elements of interest. The selected alloys were single- and two-phase structures in the Ni-Cr,6 Ni-Mo,7 and Ni-w 8 systems. The alloys were vacuum melted and cast, utilizing high-purity raw materials, in the form of 15 lb ingots. They were readily forged into 1/2-in. bar stock (except the two highest chromium alloys). The alloy compositions are shown in Table I. Typical impurity values are: Carbon: Max 0.03 pct (except for 30 and 35 pct Cr alloys which had 0.07) Nitrogen: Max 0.005 pct (except for two of the Cr alloys which had 0.05) Sulfur: Max 0.004 pct Silicon: Max 0.05 pct Each alloy was solution treated (air quenched) to produce comparable grain size. The two-phase alloys were then overaged in an effort to produce a stable structure for testing at 1200° and 1500°F, The results are summarized in Table 11. Following the heat treatments outlined in Table 11, the bars were machined to a gage section of 1.25-in. long by 0.250-in. diam. In addition to room-temperature tensile tests, stress-rupture tests were run at 1200" and 1500°F for time periods from 0.1 to about 500 hr. RESULTS Room-Temperature Mechanical Properties—The ultimate tensile strength, total elongation, and reduction of area values for all the alloys are plotted vs atomic percent of the solute element in Fig. 1. It can be seen that for the same amount of solute element the ultimate tensile strength increases in the order chromium, molybdenum, tungsten. Elongation increases (reduction of area decreases) with increasing amounts of solute for all the solid solution alloys, the values ranging from 50 to 70 pct. The ultimate tensile strength values for the two-

Jan 1, 1961

By L. D. Jaffe

IN 1945-1946, the author measured temper brittle-ness in ingots of varying composition prepared by remelting SAE 3135 bar stock under vacuum. Since other investigators1-" have been referring to this hitherto unpublished work, belated publication seems worthwhile. Steel in 7 lb batches&apos; was induction melted with nickel additions in a magnesia crucible under a pressure of 10 microns of Hg or less and cast into a 2 in. diam chill mold. The compositions of ingots A, B, and C prepared in this way are shown in Table I; the vacuum melting lowered carbon, manganese, sulphur, and nitrogen content. Ingot B was homogenized 24 hr at 1095°C; ingots A and C were not homogenized. Blanks, M in. square, were cut from each ingot, austenitized 1 hr at 870°C, water quenched, tempered 1 hr at 595"C, and water quenched. Half the blanks from each ingot were given an embrittling treatment of 50 hr at 455°C and water quenched. A few specimens, embrittled and unembrittled, were finally heated 1 hr at 580°C and water quenched. Charpy specimens machined from the blanks were V-notched on the side closest to ingot mid-radius and paired as to radial position in the ingot, one of each pair having received the embrittling treatment and the other not. Specimens were broken in a standard impact machine at various temperatures, the same temperature, in general, being used for both bars of a pair. Fig. 1 shows the results. It is evident that temper brittleness, as measured by the increase in temperature of transition from brittle to tough failure introduced by the 455°C treatment, was decreased but not eliminated by reducing carbon to 0.006 pct, manganese to < 0.004 pct, and nitrogen to 0.001 pct. In another study," temper brittleness was apparently eliminated by -reducing carbon to 0.003 pct, with 0.80 pct Mn and 0.0015 pct N (ingot D)." • Analyses given for carbon below 0.02 pct were made by Jensen method; for nitrogen, by Kjehldahl method. Values quoted else-where&apos;-&apos;." for carbon content of ingot C and for nitrogen content of ingot D were obtained by conventional combustlon and by vacuum fusion methods, respectively, and are considered much less accurate. The 580°C final treatment removed previous em-brittlement (ingot B particularly), indicating that this was "reversible embrittlement."" Metallographic examination of ingot C with 1 pct nital etch revealed only ferrite; ingot A had carbide spheroids uniformly distributed in a ferrite matrix. With ethereal picric acid plus zephiran chloride etchant.&apos; no differences between embrittled and un- embrittled specimens of ingots A, B, or C were noted. Fracture of C and D below the transition temperature was predominantly transcrystalline, with traces of intercrystalline, in both embrittled and unembrittled conditions. The corresponding fracture of unembrittled B was mixed transcrystalline and intercrystalline; of embrittled B, predominantly intercrystalline with some transcrystalline areas. . . . Acknowledgment The efforts of J. C. Leschen, formerly of National Research CO~P., in preparing the ingots are acknowledged with thanks.

Jan 1, 1956

By G. B. Craig, H. E. Rosinger, W. J. Bratina

NUMEROUS studies have been reported on how the mechanical properties of a bcc metal are affected by interstitial solute atoms in the temperature range where appreciable diffusion occurs in finite time. Only recently, though, has work on an "interstitial-free" iron been reported, this by Leslie and sober,&apos; on an Fe-0.15 pct Ti alloy. The data was limited to a maximum temperature of 296°K. This work presents a systematic study of the flow stress and the activation volume of a similar material as a function of plastic deformation over the temperature range 253" to 473°K. The material studied was Ferrovac E iron containing 0.01 wt pct C and 0.0002 wt pct N annealed at 870°C for 1 hr, and the same iron with an addition of 0.15 wt pct Ti annealed at 870°C for 80 hr; cooling rates being 75°C per hr. In the latter alloy depletion of interstitials in the a-iron matrix associated with the second phase formation was expected. The temperature dependence of the flow stress was measured at 6 = 3.33 x 10-5 sec-1 from 253" to 473°K as a function of the deformation in 0.01 intervals from 0.03 to 0.12 strain. Results for two strains, 0.03 and 0.09 are shown in Fig. 1. The flow stress increased and reached a maximum in the Ferrovac E iron with increasing temperature, but showed a consistent gradual decrease in the Ferrovac E-0.15 pct Ti alloy. A yield point and Luders region, observed in Ferrovac E, was absent in the Ferrovac E-0.15 pct Ti alloy. Also, the Ferrovac E exhibited a serrated stress-strain behavior in the temperature range 330" to 400°K; dynamic strain-aging characteristics were absent for the titanium alloy. The activation volume was determined over the same temperature range by the method of stress relaxation at constant strain. Results are shown in Fig. 2. At the temperatures of serrated stress-strain behavior in Ferrovac E the activation volume was found to increase toward infinity and, as the temperature rose, to decrease, to about 100 to 200 v/b3. By contrast, the activation volume for the Ferrovac E-0.15 pct Ti alloy tended to increase continuously from the initial value of approximately 300 at 300°K to more than 800 at 473°K. Above 400°K, then, the corresponding activation volume values of Ferrovac E were less than that of the Ferrovac E-0.15 pct Ti alloy. The activation volumes, Fig. 2, appear to depend on dislocation-interstitial interaction in Ferrovac E and on dislocation-dislocation interaction in Ferrovac E-0.15 pct Ti alloy. The gradual increase in the latter metal is associated with thermally activated motion of dislocation segments.&apos; The decrease of the activation volume in Ferrovac E above 400°K is probably related to the diminishing effect of interstitials on dislocations. Here, the interstitials can be moved along with a dislocation without appreciable drag. As indicated in Fig. 1, removal of interstitials

Jan 1, 1970

By E. T. Stephenson

Wert and Marx1 pointed out that a straight-line relationship exists between the activation energy of a relaxation process and the temperature at which the maximum relaxation occurs. The data available at the time indicated that this relationship held for a number of Snoek peaks, several grain boundary peaks, and pair relaxation in a brass. Theoretical justification for the observed relationship was found in the following equation, which Wert and Marx derived from the theory of interstitial atomic diffusion coefficients:&apos; where AH is activation energy, R is the gas constant, T is the internal friction peak temperature, v is the interstitial atomic frequency, f is the frequency of the applied stress, S is entropy of activation. More accurate internal-friction data on interstitial diffusion in bcc metals have become available since Wert and Marx&apos;s paper. Table I gives activation energies calculated by several authors from a combination of elastic aftereffect data and the peak temperatures at several frequencies of measurement. (In the case of Fe-C and Fe-N, the referenced authors5&apos;7&apos;8&apos;10 also used high-temperature diffusion data.) However, diffusion experiments at 150°C and above1&apos;-13—rather than anelastic techniques—were used to determine the activation energy of hydrogen diffusion in Fe-H. In order to plot this recent data as a AH vs T graph we calculated the peak temperatures of the systems listed in Table I (with the exception of Fe-C, Fe-N, and Fe-H) by using published values3&apos;&apos; of AH and Do. These calculated peak temperatures varied by only a few degrees from experimentally determined peak temperatures. The calculated values were felt to represent the better average. A number of investigators have found the peak temperatures in Fe-C and Fe-N to be 38 to 40°C and 20° to 24°C, respectively. The values of 39" and 22°C (312° and 295°K in Table I) were determined by carefully executed experiments.6&apos;8 The hydrogen peak temperature has been measured at 1 cps,12 20 cps,14 and 35,000 cps.15 All hydrogen peak temperatures were adjusted to 1 cps for Table I using AH = 3000 cal per mole. As Fig. 1 shows, the data of Table I fit a straight line at least as well as the earlier data used by Wert and Marx. Linear-regression analysis was applied to the data in Table I. The Fe-H data was omitted because the activation energy has not been experimentally determined in the temperature range of the peak. The analysis yields the equation: with a standard error of 860 cal per mole. The agreement of the data in Table I with the Wert-Marx equation is excellent. Strict application of Eq. [I] forces the linear regression analysis through the origin. In this case, the analysis gives a slope of 62.1 cal per mole per deg, and a standard error of *890 cal per mole. With this value, it follows from internal-friction theory that Hence, Do varies by only 30 pct among these bcc-interstitial systems. Thus, a concept suggested originally by Wert and Marx1 is confirmed by recently published data. The

Jan 1, 1965

By H. Siebel, N. A. D. Parlee

MIZIKAR, Grace, and parlee&apos; studied rates of absorption of oxygen in stagnant liquid silver in a new type of open-ended gas-liquid metal diffusion cell, where the capillary diameters used were 1.5, 2, and 3 mm. They reported that the rates appeared to be controlled by the rate of diffusion of oxygen atoms in liquid silver and they used their data to arrive at the following equation as a reasonably good representation of the diffusivity (D) of oxygen in liquid silver: D = (14.7)10-4 exp (-7100 ± 3200)/RT cm2/sec Since this type of diffusion cell offers a promising method of measuring diffusivities of gas atoms in liquid metals, the senior author of this note and his students are carrying on a critical examination of the method, and are attempting to improve and extend the technique. The research reported briefly here was designed to examine more carefully the earlier conclusion1 that the absorption rate is diffusion-controlled, and to find out whether the diameter of the cell could be greatly increased and thus extend the method to systems where gas solubilities and diffusion rates are much smaller than in the case of oxygen in silver. For the purpose of these experiments, the open-ended capillary cell used by Mizikar, Grace, and Parlee was replaced by a small cylindrical crucible (1 to 1.7 cm in diam) containing pure silver (to a depth of 1.3 to 3 cm) resting in the bottom of a closed-ended vertical quartz tube, with an evacuated quartz filler tube just above the crucible to reduce dead volume. The method of measuring the rate of absorption was otherwise very similar to that of Mizikar, Grace, and Parlee and all the same precautions were taken. A much smaller and shorter tube furnace was used for heating, but simi- lar precautions about temperature gradients were observed. This technique was nothing more than the application of a Sieverts apparatus to the measurement of rates of absorption in small crucibles of stagnant liquid silver. In each run the volume of gas absorbed (V) was plotted against the square root of time (vt) and apparent diffusivities were calculated from the slope of the line, as described by Mizikar, Grace, and parlee.&apos; Care was taken to use only the data obtained during the early part of the total absorption period while the cell functioned as one of infinite depth. The results at 1000°C are summarized in Table I and Fig. 1. The following conclusions may be drawn: 1) Diffusion cells up to 1.7 cm in diam yield, within experimental error, the same values for the diffusivity of oxygen (D) as the capillary cells of 1.5, 2, and 3 mm in diam employed by Mizikar, Grace, and Parlee. Cell diameters as large as 1.7 cm are probably not desirable for the most precise work. Intermediate sizes, perhaps 0.5 cm, will be most practical. 2) All absorptions measured were consistent with a model where the rate is controlled by the diffusion of gas atoms in the metal. The fact that runs at absorption pressures ranging from 0.1 to 1 atm (at any one temperature) give

Jan 1, 1965