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By K. M. Rolls, F. W. Reuter, J. Wulff

The superconducting behavior and microstructural characteristics of a nominal Nb-40 wt pct Ti-0.239 wt pct O alloy were studied as a function of ther mo -mechanical processing treatment. Critical current density us applied transverse magnetic field was obtained for 0.010-in.-diam wires at 4.2°Kin steady fields 14 to 110 kG. Both optical metallogvaphy and transmission electron microscopy were used to delineate the micros tructures of the same wires. It wan found that a 1-hr 500°C precipitation heat treatment after cold drawing to final size led to the highest critical current density. Heat treatment at 600°C also led to a high critical current density, but the precipitate differs in kind and form from that at 500°C. The resistire critical field was also found to be sensitive to precipitation heat treatment since the effective composition of the superconducting phase changes. This is discussed in terms of the oxygen in interstitial solid solution. Two types of high-field superconducting wire are at present used in the construction of high-field superconducting solenoids. These types are solid-solution alloy wire such as Nb-Zr and Nb-Ti and composites of the brittle inter metallic compound Nb3Sn. The latter generally have a high super cur rent-carry ing capacity which is difficult to vary if properly made. The supercur rent- carry ing capacity of the former can be varied drastically and often predictably by suitable thermomechanical processing treatments. In general, the critical current density Jc of the solid-solution type of alloy is increased by cold work and by additions of interstitial elements along with aging heat treatments. The imperfections which result are be-iieved to be responsible for the observed increase in Jc. In 1962 Kneip and coworkers1 found that the critical faurrent density of Nb-Zr alloys could be increased by proper heat treatment preceded and followed by cold work. Betterton and coworkers2 using a Nb-25 at. pct Zr alloy found that small additions of oxygen or carbon enhanced the effect of this heat treatment. They suggested that the interstitials present aided precipitation in the alloy, leading to a filamentary structure with superior properties. If the precipitation heat treatment was omitted, interstitial additions had a negligible effect on Jc. wong3 showed that higher heat-treatment temperatures lowered Jc. Walker and co-workers,4 who studied microstructure (by transmission electron microscopy) as well as superconductivity, found that the Jc anisotropy introduced by cold rolling was itself affected by heat treatment. They were unable to clarify the relation between microstructure and critical current density, although evidence of precipitation was indicated. More recent investigation of Nb-Zr alloys,5,6 besides showing that structural defects and fiber ing due to cold work and precipitation serve to raise Jc, also elucidate important optically observable microstructural changes which occur upon precipitation. In these reports, coarsening of the microstructural features was found to decrease Jc. Vetrano and Boom,7 who studied Ti-20.7 at. pct Nb, found that Jc was increased to a maximum by a 415°C, 3-hr heat treatment following quenching from 800°C and cold working. Heat treatments can also affect the resistive critical field Hr. Final-size heat treatments of Nb-Zr wire can lower Hr drastically if gross phase decomposition occurs5'* or moderately if the effects of cold work are eliminated without changing significantly the composition of the phase of interest.3,5,6,8 The percentage of oxygen which can be added to Nb-Zr alloys to enhance Jc is limited by the difficulty of subsequent cold drawing. Since Nb-Ti and Ta-Ti alloys in contrast can tolerate appreciably higher percentages of oxygen, it was decided to investigate the superconducting behavior of various alloys in these systems. The present paper describes the results of adding oxygen to a nominal 40 wt pct Nb alloy as a function of thermomechanical treatment. I) EXPERIMENTAL PROCEDURE A small alloy ingot was prepared from high-purity niobium, iodide, crystal-bar titanium, and Nb2O5 powder by arc melting on a water-cooled copper hearth in a gettered argon atmosphere. The ingot was turned and remelted fourteen times to insure homogeneity. After final melting and rapid cooling, it was machined round to 0.415 in. diam, jacketed in stainless steel, and cold-swaged to 0.117 in. diam. The jacket was removed and swaging continued to 0.051 in. diam followed by wire drawing in carbide dies to 0.010 in. diam. Although it was intended that about 1500 ppm O (by weight) be added, inert gas fusion analysis indicated a 2390 ppm 0 content, apparently due to additional oxygen pickup in the arc furnace. Even so, the alloy was sufficiently ductile to be cold-worked to greater than 99.9 pct reduction

Jan 1, 1967

By R. P. Abendroth

The hydrogen-water vapor ratio at which Fe-Cr alloy, chromium oxide, andiron chromite coexist in equilibrium was determined between 900" and 1200°C. A thermogravimetric method was used to determine equilibrium conditions. The results fit a straight-line relationship in the temperature region studied, and are given by Reduction experiments were also performed to confirm the results of the equilibrium investigation. ThE oxygen pressures at which Fe-Cr alloy, chromium oxide, and iron chromite coexist in equilibrium have been previously determined by Boericke and angert,' Morozov and Novokharski,' and Katsura and uan. Only one determination (at 1300°C) was made by Katsura and Muan, but it agrees with the results of orozov and Novokharski. The results of Boericke and Bangert, however, differ appreciably from the results of these investigators. Previous studies have assumed that the equilibrium metallic phase is pure iron, but Dahl and Van vlack have shown that the iron contains from about 1 wt pct Cr at 1000°C to over 2 wt pct above 1300°C. The chromium oxide also contains a small amount of iron in solid solution. In the present study, hydrogen-water vapor mixtures were equilibrated with the condensed phases, using a therrnogravimetric method to determine equilibrium conditions. The reaction can be written EXPERIMENTAL General Procedure. The starting material was a sintered pellet of Fe2O3-Cr2O3 solid solution with a hole in the center, and was placed on a fused silica hook. This assembly was raised into the preheated hot zone of the furnace in a helium atmosphere, hooked onto a fused silica hangdown suspended from one arm of an Ainsworth Model RV-AU-1 recording balance, and the starting weight determined. A flowing hydrogen-water vapor atmosphere was then exchanged for the helium by evacuation, and the sample reduced until the weight loss indicated the sample composition to be in the alloy-Cr2O3-chromite field. The tem- perature was adjusted incrementally until constant sample weight was achieved for several hours, to within 0.02 mg. A hydrogen-water vapor atmosphere of different composition was then admitted, and the same procedure carried out. At the end of a series of determinations, the sample was examined by X-ray diffraction to verify the presence of the desired phases. Microscopic examination of the silica hook showed no interaction with the sample, nor did it lose any weight. Several criteria were used to insure equilibrium besides constancy of weight. For a given hydrogen-water vapor composition, equilibrium was approached from both oxidizing and reducing sides by varying the furnace temperature slightly. The resulting slow weight loss or gain was observed for several hours. Constant weight could be re-established by returning to the original furnace temperature. The last criterion used was varying the relative amounts of the phases by further reduction or oxidation, and observing any changes in temperature required for constant weight for a given hydrogen-water vapor atmosphere. None were observed. This procedure was essentially the same as approaching the equilibrium from oxidizing and reducing sides, but larger weight excursions were carried out. Sample Preparation. Reagent-grade Fe2O3 and Cr83 powders were mixed in the desired proportions and heated in air at 1250°C for 2 hr. The mixture was re-ground and heated in air overnight at 1250°C. X-ray diffraction showed complete solid-solution formation as a result of this procedure. The solid solution was then pressed into l/2-in.-diam pellets using Carbowax 4000 as a binder. The hole was drilled in the center, and the pellets were sintered 24 hr at 1250°C in air on a bed of Fe2O3-Cr2O3 of the same composition, contained in an alundum boat. After cooling, the pellet surfaces were abraded with 310 paper to remove any surface compositional differences, such as loss of Cr2O3. Chemical analysis of the sintered pellets was 67.16 wt pct CrP3 and 33.02 wt pct Fe203. Atmosphere Generation and Control. The hydrogen-water vapor atmospheres were generated by passing Matheson ultrahigh-purity hydrogen, with no further purification, through two water bubblers contained in a constant-temperature water bath. Since the water-vapor dew points required in this study were below room temperature, the bath was insulated, and was cooled by thermoelectric-immersion devices. The bath temperature was controlled to 0.0l0C. Since rather high flow rates of about 900 ml per min were used through the furnace tube, an independent check of the dew point was made to insure saturation of the hydrogen by the water vapor. Although the dew point could only be determined to within 1/2"C, the determined dew points agreed with the water-bath temper-

Jan 1, 1967

By Stanley A. Feitler

This Bureau of Mines report deals principally with the resources and economic aspects of feldspar in the United States east of the Mississippi River. Although in a strict sense, all phases of the feldspar industry affect its economic structure, emphasis in this study is on supply, demand, and marketing. Although feldspar was originally mined for use in the manufacture of pottery and other ceramics, the glass industry, which began to use feldspar in the mid-1920's, now consumes more than half of the annual output. Most mining is open cut, and the methods used are similar to those used in mining crushed stone. Excess plant capacity has been chronic, and production is usually about 50 percent of capacity fur the industry as a whole. Since 1947, feldspar consumption has grown more slowly than the average for all U.S. industry. This has fostered intense competition, especially for the glass market. Prices have not kept pace with inflation, and profits are small. The trend of consumption through 1.970 for glass feldspar is expected to be upward; less rapid growth in consumption of ceramic feldspar is anticipated.

Jan 1, 1967

By G. A. Parks, C. Kovacs

The xanthate flotation of chrysocolla can be improved by preheating the ore to 500° to 600°C. Addition of water vapor reduces the preheating temperature required. The temperature range of flotation improvement correlates well with the range over which dehydroxylation occurs. This observation is consistent with changes in the structure and properties of the mineral as detected by measurement of solubility, D.T.A., T.G.A., X-ray diffraction, and infrared absorption and with recently proposed explanations of chrysocolla flotation. A brief experiment by one of the authors several years ago showed that exposure of chrysocolla to high temperature water vapor resulted in increased recovery by subsequent xanthate flotation. Recently renewed interest in flotation and thermal properties of chrysocolla1-5 prompted further study of this effect and more detailed reporting.6 This paper explores the response of pure chrysocolla recovery in Hallimond tube flotation tests to the time and temperature of exposure and to changes in the water vapor pressure. Brief attention is paid to the effects of such treatment on accessory minerals. A single experiment with flotation of chrysocolla from an ore is reported. MATERIALS Chysocolla from Inspiration, Gila County, Ariz. was crushed in a porcelain mortar, cleaned of visible and magnetic impurities, and screened to obtain -48 +65 mesh (Tyler) material for flotation test work. The clean material contained 28.5% Cu and was identified as chrysocolla by comparison of X-ray diffraction, D.T.A., and infrared absorption data with that reported for similar materials by others.4,5,7 Samples of malachite and chalcopyrite, prepared in a similar way, were also identified by X-ray diffraction. The sources of these materials are unknown. A sample of chysocolla-bearing oxidized copper ore from Pima, Ariz. was crushed and dry ground for thermal activation and subsequent flotation. PROCEDURES Activation: The apparatus used for exposure of materials to high temperature water vapor is illustrated in Fig. 1. The furnace temperature was controlled to ±5°C Water vapor pressure was controlled by pre-saturating a nitrogen carrier stream with water in an adjustable thermostatted saturator (multiple bubbler). A water manometer and capillary orifice flow meter were used to measure nitrogen flow rates for activation and for subsequent Hallimond tube tests. Gas flow rate and temperature were adjusted prior to introduction of samples. Exposure time was measured from the moment of introduction of the sample to the furnace, hence includes an initial drop below the control temperature. After heating, the samples were removed from the furnace and stored at room temperature in air. Representative samples of activated materials were examined by X-ray diffraction and infrared absorption.

Jan 1, 1967

By Edward A. Vitunac

The emerging importance of pneumatic conveying systems for bulk materials is becoming recognized by more persons responsible for materials management as consultants, at the corporate level and at the plant level. They have learned that the economic advantages of a pneumatic system are frequently decisive when compared to alternate methods. Included in these advantages are relative simplicity, ease of installation, flexibility, ease of maintenance, cleanliness, safety and ease of automation to the degree desired. In general, installed costs favor a pneumatic system when compared to competing mechanical systems if the transporting distances are long or to and from many points. In addition, supplemental use such as cooling, heating, or drying may supply the incremental value required to justify its selection. (1). The main disadvantages of a pneumatic system is the greater horsepower required per unit weight of material conveyed and material limits in abrasiveness and density. In addition, there is a tendency to increase material breakage at changes of direction and at any obstruction such as the imperfect butting of one, piece of pipe to another in the conveying line. Classification of the material at the discharge may also cause problems in dusting and segregation. Materials weighing less than 4 pounds per cubic foot tend to cause feeding and collecting problems although they can be conveyed easily. Material between 4 and 20 pounds per cubic foot can be handled with less problems but flow rate is hard to predict. The 20 to 60 pounds per cubic foot range offers best results; whereas, over 60 pounds per cubic foot, materials tend to drop out of the air stream and settle in the pipe line unless careful provisions are made to prevent it. (2).

Jan 1, 1967

By Keith K. Griffiths

Computers are a valuable tool to the aggregate industry and should not be overlooked. The selection of proper mechanical components is necessary. Merely the addition of a computer to operate a mechanical system will not guarantee that the system will work. Material delivery by rail or truck for stock-piling and intra-plant material transfer can be accurately supervised by automation with simplified controls for the layman to use. There are mechanical problems that occur in material blending and load-out systems when such a system is automated. Such things as material flow, bridging, stockpiling methods, overloading of equipment and safety must be considered. How these problems can be overcome by proper selection of compatible mechanical and computer equipment will be discussed. Also, there are many individual material circuits in a plant that can be computerized at a nominal cost. This type of computer installation will not necessarily result in increased production, but it will produce greater efficiency in manpower. These small computers, binary counters, memory circuits and other devices and their application to the aggregate industry will also be presented. A careful evaluation of the mechanical and computer inter-relationship by someone understanding both "Rocks and Electronics" is essential to proper handling of material by computers. Computers for the mining industry may be either digital or analog computers. Unless the computer is to control some type of chemical process, such as a cement plant, the, analog computer is not required and the digital computer' will be quite adequate and less expensive.

Jan 1, 1967

By G. W. Phelps

The field of industrial minerals is concerned with both sieve size and distribution of sub-sieve particles. A great deal of work has been reported on the techniques designed to provide information of this work. The term sub-sieve is here considered to include particular material that will pass a 325-mesh testing sieve. Plant men require rapid, precise and simple testing techniques that are, if possible, inexpensive with respect to equipment and manpower. A number of particle-size procedures have been developed, based on the Stokes equation for streamline movement of a particle of diam D, moving at velocity V through a liquid of viscosity n. 1 Particles are considered to be rigid, smooth spheres, completely dispersed at low concentration and moving at low velocity through the suspending medium with no slippage between particle and liquid. In particle size determinations the particle moves either from natural gravitational forces or those provided by centrifugal means. The diagram of Fig. 1 shows a spherical particle of density S and diam D moving downward at velocity L/T (or V) through a liquid of density So and viscosity n. The forces of gravity G (natural) or Gc (centrifugal) cause the particle to move through the liquid, thereby creating a viscous drag F or Fc. Within the streamline flow

Jan 1, 1967

By M. J. Lempel

A theoretical study of the heat-transfer characteristics of a dilute gas-solids mixture in an externally heated tube is reported. Detailed equations are developed describing the system, and a numerical method is presented to solve the equations using a digital computer. The methods are applied to a system containing fine coal particles entrained in hydrogen, flowing through a hot tube. Heat-transfer coefficients and several other physical constants are evaluated in detail.

Jan 1, 1967

By Edmond F. Lawrence

The Calico area lies within the Walker Lane fault zone, six miles north of Schurz, Nevada. The mineralized area is overlain by a thick section of Tertiary tuffs and ash-flows, that have been intruded by a series of andesite plug, dikes, and sills. The pre-Tertiary rocks outcrops only in two areas at one to two miles distance from the drilling areas. Underlying the volcanics are sediments ranging from siltstones, sandstone, calcareous shales, to carbonates of the Luning sequence. These have been intruded by one or more phaneritic intrusives ranging in composition from quartz diorite to quartz monzonite, with the development of a skarn zone on the south flank that contains extensive mineralization consisting of magnetite, pyrrhotite, pyrite, and chalcopytite, with traces of sphalerite, galena, and molybdenite. The magnetite, pyrrhotite, and part of the pyrite appears to be contemporaneous with the skarn, while, part of the chalcopyrite, galena, sphalerite, molybdenite, quartz, and calcite, occurs as minute veinlets cutting the other minerals. This later mineralization may be associated with a late stage of the same sequence, or possibly associated with another intrusive to the southwest. Geophysical work has consisted of aerial magnetics, ground magnetics, gravity, seismic, and induced polarization surveys. Preliminary induced polarization surveys indicated anomalies at depth, both over the magnetic anomaly and to the northwest. Subsequent IP work confirmed this earlier anomaly, and drilling disclosed extensive mineralization at depths of 400 feet on the northwest end and over 1,000 feet to the southeast.

Jan 1, 1967

"Many advances in glass technology and processing are being made and the possibilities for glass as a material in the future appear unlimited. Float glass, glass-ceramics, high-strength sheet and container glass, glass-reinforced plastics, glass for electronic equipment, aerospace glass, glass fibres, glass vehicles, glasses with selective-reflective coatings and glare-reducing glasses, to name a few, provide areas of significance at present and for the future. There appear to be great opportunities, in certain localities of Canada, to develop new sources of raw materials for an expanding Canadian glass industry.New developments in the structural clay products industry have centered around facing brick as a structural load-bearing material, prefabricated brick panels, large-sized units, isostatic pressing of sewer pipe and auto-matic settmg of brick. Fast-firing techniques, using prefired or calcined raw materials, and the development of high-strength products will result in the use of a wider range of raw materials in the whiteware and structural clay products industries.Porcelain enamel, a material used for many years in domestic appliances and for sanitary ware, now is used extensively in architecture, agriculture, water tanks, highway signs and reflectors, and in products where resistance to corrosion-plus-temperature is important. Exotic composites of ceramics and metals, and specialized ceramic coatings applied on metals by various techniques such as flame spray, plasma jet, or vapour and chemical deposition have proved useful in materials for aircraft power plants, rockets, missiles and nuclear applications."

Jan 1, 1967

By O. M. McRae

The Courtland-Gleeson area is in Cochise County about 15 miles east of Tombstone in southeastern Arizona. Rocks exposed in the area range in age from Pre-cambrian to Quaternary. The Precambrian is repre-sented by the Pinal schist. Paleozoic rocks include the Cambrian Bolsa quartzite and Abrigo limestone, Mississippian Escabrosa limestone, and the Permo-Carboniferous Naco Group limestones. Rocks believed to be of Triassic and/or Jurassic age include the Copper Belle monzonite porphyry, Turquoise granite, and Gleeson quartz monzonite. The Cretaceous is represented by andesitic volcanics and various sedimentary rocks. Tertiary rocks include the intrusive and extrusive Sugarloaf quartz latite porphyry and numerous dikes of various rock types. Quaternary conglomerates cover the northern and eastern part of the area. The geologic structure is extremely complex. All rocks as old as early Tertiary have been involved in either tilting, normal faulting, high angle reverse faulting, imbricate thrusting or folding and overfold-ing. Major deformation was initiated during the first half of the Tertiary. Northeast-southwest compres-sional forces caused thrust plates containing lower Paleozoic rocks to override Cretaceous rocks. Subsequently, two large slide blocks of lower Paleozoic rocks, acting under the influence of gravity, moved eastward. The imbricate structure and the gravity slide blocks were then broken by late Tertiary normal faults. INTRODUCTION The Courtland-Gleeson area, or Turquoise Mining District, has long been recognized as an area of extreme structural complexity. Gilluly 2 referred to the entire district as a "gigantic thrust breccia". In 1962, Bear Creek Mining Company completed a two year program of detailed geologic mapping supported by exploration drilling. The purpose of this paper is to present some of the results of this investigation and to provide a structural interpretation based on these results. The geologic map that accompanies this report is generalized and shows only the major and significant features. The area was initially mapped on aerial photographs on a scale of 1 in. equals approximately 500 ft. These data were transferred to a planimetric base using a vertical sketch master. LOCATION The Courtland-Gleeson area is in central Cochise County, about fifteen miles east of Tombstone, and about twenty-two miles northeast of Bisbee in southeastern Arizona (Fig. 1). The area is readily accessible over graded gravel roads from both Tombstone and Elfrida. GENERAL GEOLOGY Rocks exposed in the area range in age from Pre-cambrian to Quaternary. wilson3 and Gilluly2 have published very detailed descriptions of the principal rock units exposed in the area. Only a summary description is provided in Table I. A great number of previously unmapped narrow Tertiary dikes and small irregular masses of hornblende andesite porphyry, lamprophyre, and aplite intrude the Gleeson quartz monzonite in the western part of the map area. The scale of the map prohibits showing them. The aplite dikes are related to, and bear the same structural relationships as, the Sugarloaf quartz latite dikes found in this area. For that reason, and because both the hornblende andesite porphyry and the lamprophyre are post-mineral and post-thrusting, their omission from the map is not considered significant. Because so many of the contacts in the district are fault contacts, because bedding faults appear to be prevalent but are difficult to recognize and map, and because igneous intrusions are so common throughout the sedimentary section, it is virtually impossible to measure an exact total thickness of any of the sedimentary rock units. Nevertheless, neither the field mapping program nor the diamond drilling provided any basis for suspecting that the thicknesses of the sedimentary units are significantly greater or less than what might be inferred from surrounding districts.

Jan 1, 1967

By A. P. Fletcher, K. Croteau

The intent of this paper is to cover some aspects of preventive maintenance methods which have come into wider usage in recent years as a means of increasing operating efficiencies. Particular emphasis is placed on lubrication and related servicing.

Jan 1, 1967

By E. A. Zawadzki

The problem of pollution of water by mine drainage is at least as old as the mining industry itself. However, research on the formation, composition, treatment, and abatement of mine water is a relatively recent historical event. At Bituminous Coal Research, Inc., acid mine drainage control has been an important area of work since 1944, at which time BCR began sponsorship of research at West Virginia University. The work at West Virginia University involved a detailed study of the acid mine drainage problem and led to the identification of iron oxidizing bacteria as important factors in the formation of acid mine water. The results of this research were summarized in 1954 by Temple and Koehler (1) who concluded that "no practical solution for the problem" of controlling acid mine drainage is yet known.?

Jan 1, 1967

By R. M. Waterstrat, E. C. van Reuth

BINARY- alloy phases having the A15-type crystal structure have been described as occurring at a simple and more or less invariant stoichiometric composition (A3B) which corresponds to the relative number of atoms occupying each of the two crystallographi lattice sites in this structure.1,2 It is frequently assumed, therefore, that each crystallographic site is occupied exclusively by one kind of atom. In most cases, however, there have been insufficient experimental data to establish whether atomic ordering is, in fact, complete. Recent studies have shown that binary A15-type phases are sometimes stable over an appreciable composition range3''* and, occasionally, the composition range of stability does not even include the "ideal" A3B stoichiometric composition.5-7 We have observed the existence of nonstoichiometric A15-type phases in the binary systems Cr-Pt and Cr-Os. This has not been reported in previous work on these alloy systems.1,8-11 A series of alloys, each weighing approximately 30 g, was prepared by are-melting in an Ar-He atmosphere using 99.999 pct Cr, 99.999 pct Os, and 99.99 pct Pt as starting materials. Each alloy was melted four times with a total weight loss of less than 1 pct. The stoichiometric (A3B) alloys were sealed in evacuated quartz tubes and annealed at 1200°C for periods of time ranging from 3 days to 2 months. Examination of the alloy microstructures revealed that little change had occurred over this time interval and it was therefore assumed that the microstructures were fairly representative of equilibrium conditions. No evidence of contamination was observed although there was apparently some loss of chromium which was confined to a thin layer at the surface of the specimens. The quartz tubes were quenched from the annealing temperature into cold water. X-ray diffraction and metallographic examination of the stoichiometric alloys revealed an estimated 10 to 30 pct of second phases which were tentatively identified as phases previously reported in these binary-alloy systems.8-11 A second series of alloys was prepared by mixing -325 mesh metal powders having a nominal purity of 99.9 pct and compressing these mixed powders in a cylindrical die at a pressure of 43,000 psi. These alloys, each weighing 15 g, and some of the arc-melted alloys were annealed in a high-temperature vacuum furnace heated by tantalum strips at a pressure of 10-8 Torr and were rapidly cooled by turning off the furnace power. X-ray and metallographic examination of both series of alloys served to establish the composition ranges of the A15-type phases. Although some chromium losses occurred during the vacuum annealing, they were largely confined to a thin layer on the outer surfaces of the samples. It was established that the A15 phases occur in the Cr-Pt system at 21 ± 1 at. pct Pt after 1 week at 1200°C and in the Cr-Os system at 28 ± 1 at. pctOs after 1 day at 1400°C (see Table I). We also observed that an arc-melted stoichiometric (A3B) alloy in the Cr-Ir system was single-phase (A15-type) in the "as-cast" condition in agreement with previous work.8,13 In addition we obtained a sample of the Cr-Os A15-type phase from Argonne National Laboratory. This alloy contained less than 1 pct second phase12 and was submitted to a density measurement. The density measurement yielded a value of 11.14 g per cu cm in comparison to a theoretical value of 11.25 g per cu cm calculated using the observed lattice constant (4.6806Å) of this alloy. The uncertainty in measurement was 0.1 pct but the sample may have contained some cracks or minor imperfections which could account for the low experimental value. We have also studied the atomic ordering in these phases by means of integrated line intensity measurements using thick, flat, rotating powder samples and CuK a radiation in an X-ray diffractometer. We have obtained order parameters of 0.90 for the Cr-Pt phase, 0.89 for the Cr-Ir phase, and 0.64 for the Cr-Os phase using the formula: where s is the usual Bragg and Williams order parameter, ra is the fraction of chromium atoms in A sites, and FA is the fraction of chromium atoms in the alloy. The values obtained are estimated to be accurate within ±4 pct. If the unusually small value for the order parameter of the Cr-Os A15 phase were due to the existence of lattice vacancies on the "B-atom" sites, then a density of 10.04 g per cu cm would be expected in contrast to the observed value of 11.14 g per cu cm. We, therefore. conclude that the fraction of lattice vacan-

Jan 1, 1967

By T. Kessler

The purpose of this investigation was to evaluate the application of a spark-source mass spectrograph equipped with a spinning-electrode system for the study of various high-molecular-weight materials derived from coal. Conclusions from the investigation of anthracene, phenanthrene, chrysene, coronene, truxene, a coal-tar pitch (800 to 850 C softening point), and anthracene-chrysene synthetic mixtures follow: 1. Simplified mass spectra of anthracene, phenanthrene, chrysene, coronene, and truxene, from which the molecular weights were easily determined, were obtained by the spinning-electrode system. 2. Eight structural types having molecular weights from 178 to 252 corresponding to compounds previously observed in an electron impact mass spectrum of a coal-tar pitch sample were affirmed by this technique. 3. Mass spectra obtained from synthetic mixtures of anthracene and chrysene demonstrated that the technique is applicable for semiquantitative analysis.

Jan 1, 1967

By R. B. Tippin

The heavy liquid separation (HLS) process was investigated by the Bureau of Mines to develop a means of concentrating minerals from natural ores, Various spodumene ores were tested in a 0.4-inch diameter cyclone using pure tetrabromoethane (TBE) as the heavy liquid. Studies were initiated to examine the influence of (1) pulp density (2) feed grade, (3) cyclone pressure, (4) cyclone apex opening size) (5) cyclone vortex finder opening sand (6) mineral particle size on the separation efficiency. Each of these factors was found to affect the heavy liquid separation in some degree; the mineral particle size exhibited the greatest effect and the ore feed grade the least. Conditions necessary to yield an 85 percent spodumene concentrate with an 85 percent recovery were determined to be: 70 psig pressure, 10 percent solids, 0.08-inch apex opening, 0.11-inch vortex finder opening and a minimum amount of minus 200-mesh fines in the feed. Operation of multiple cyclones in series resulted in spodumene concentrates assaying over 90 percent and indicated mineral recoveries exceed-in 90 percent.

Jan 1, 1967

This report presents depth and producing rate statistics pertaining to oil reservoirs (or fields) in each of the 14 States that produced more than 20 million bbl of oil during 1965. The combined oil production was about 2.6 billion bbl, or 96 pct of the U.S. total. Data are presented for each of the 14 States, each Texas Railroad Commission district, and four geographical areas of Louisiana. About 8 pct of the total oil produced in the 14 States was from depths of lees than 2,000 ft, 24 pct from 2,000 to 4,000 ft, 22 pct from 4,000 to 6,000 ft, 16 pct from 6,000 to 8,000 ft, and 30 pct from 8,000 ft and deeper. The average production per well in the 14 States ranged from 4.4 bopd for wells less than 2,000 ft deep to 57.6 bopd for wells 8,000 it and deeper. Data indicate that 9.5 pct of the 460,968 wells produced more than 1.2 billion bbl or 46.6 pct of the total oil. Oil production from reservoirs (or fields) not undergoing stimulative recovery operations, such as steam, air, gas, or water injection, wee about 1.1 billion bbl or 42.1 pct of the total.

Jan 1, 1967

By Van E. Shaw

Fusion of an 86-percent euxenite concentrate with ammonium sulfate was investigated by the Bureau of Mines. Reaction for 4 hours at 400° C results in conversion of both the rare-earth elements and the titanium-columbium components to water-soluble compounds. Similar results are obtained with ammonium bisulfate. Stirring the fusion mass decreases the reaction time substantially. Alternatively, treating the fusion product with a 3-hour, 650° C calcining step renders the non-rare-earth constituents insoluble, thereby allowing selective leaching of a pure rare-earth fraction with an overall yield of 97 percent.

Jan 1, 1967

By F. H. Hueston, R. S. Barclay

"Depending on the application, zirconia, fused magnesia and graphite have been found to be the most suitable crucible materials for melting uranium metal and its alloys. Although graphite has been found to be satisfactory for uranium and uranium alloy castings with cross sections of 4 square inches or greater, ceramic-type molds are superior for small sections and those shaped castings which prohibit the economic use of machined graphite molds. Heating cycles, addition mechanisms and furnace conditions for melting are discussed."

Jan 1, 1967

By A. W. H. Morris, G. H. Laurie, J. N. Pratt

Using- galvanic cells of the form Sn(liq)/Sn" (LiCl-KC1-SnCl,)/Sn-Ag (alloy), measurements have been made of relative thermodynamic properties of the a, C, E, and liquid phases of the Ag-Sn alloy system. Partial heats of solution of the components in the liquid alloys lzave also been observed by direct cal-orimetric measurement in an isoperibol calorimeter. The thermodynanzic quantities are disczlssed in relation to structural and other properties and the existence of anomalous minor fluctuations in the partial heats and entropies of solution in liquid alloys is tentatively suggested. In the course of a recent electro motive-force study of the thermodynamic properties of Sn-Ag-Pd liquids,' some measurements were also performed on the Ag-Sn binary system. Most previous thermodynamic studies of this system have been concerned with the liquid state. Measurements confined to the limiting heat of solution of silver in liquid tin have been made by many calorimetric workers2 while high-temperature calorimetric measurements of the heats of formation of the full range of liquid alloys are reported in the early work of Kawakami~ (1323°K) and more recently by Wittig and Gehrin~(1248°K). Electromotive-force studies on liquid alloys have been made by Yanko, Drake, and Hovorka' (606" to 686°K; 86 to 99.4 at. pct Sn) and by Frantik and Mc Donald' (900°K; 30 to 90 at. pct Sn). The only known measurements on the solid state are of heats of formation of the a, £, and c phases; these values were obtained using tin-solution calorimetry, at 723"K, by Kleppa,~ whose investigation also yielded heats of formation of liquid alloys containing more than 64 at. pct Sn. The present experiments on the Ag-Sn alloys include a re-examination of the liquid phase and, because of the dearth of free-energy data for the solid state, attempted measurements on the a, c, and E phases. The principal new feature of electromotive-force results obtained for the liquid phase was an indication of anomalous fluctuations in the partial heats and entropies of solution of tin at certain compositions. However, since the values for these thermodynamic quantities were determined from the temperature coefficients of cell potentials, which are commonly subject to considerable error, confirmation by calorimetric measurements was considered desirable. A detailed investigation of the partial heats of solution of the components in the binary liquids was made using a liquid metal solution calorimeter. I) GALVANIC CELL STUDIES a) Experimental Details. Measurements were made, as a function of alloy composition and temperature, of the potentials of reversible galvanic cells of the form: ~n(liq)/~n++/~n-Ag (solid or liquid alloy) Details of the apparatus and experimental techniques have been given elsewhere.' so that a brief account will suffice here. Molten salt, 58 mole pct LiC1-42 mole pct KC1, containing small amounts (1 to 2 mole pct) of stannous chloride was used as the electrolyte. The salts were dehydrated by pre-electrolysis and vacuum -drying techniques. Cells were established under an argon atmosphere by immersing tin and alloy electrodes in the molten salt contained in a large silica tube, heated in a vertical resistance furnace. The tube was sealed at the top by a head plate provided with openings permitting the simultaneous insertion of six electrodes, a central thermocouple sheath, and connections to vacuum and argon lines. Temperatures were controlled to *0.2"C over prolonged periods, with maximum variation over the electrodes at any time of 0.l°C. Temperatures were measured with a standardized Pt/13 pct Rh-Pt couple. The electromotive force of this and the cell potentials were measured on a Cambridge Vernier potentiometer and short-period galvanometer. Alloys were prepared from Pass "S" tin (99.999 pct) and Johnson-Matthey high-purity silver (99.999 pct) by melting in evacuated silica capsules and quenching in cold water. For liquid phase experiments, pieces of the resulting alloys were remelted into prepared silica electrode units, while solid electrodes were prepared by remelting into 3-mm bore tubing, inserting a cleaned molybdenum lead wire, and quenching to produce uniform rods about 3 cm in length, with soundly attached leads. In all cases remelting was done under an argon atmosphere. The solid electrodes were subsequently annealed in evacu ated silica tubes for 14 days at about 20°C below the solidus and quenched. Analyses showed that these techniques produced uniform electrodes with no significant change from weighed out compositions. b) Results and Discussion. Measurements were made on about forty alloys in the solid and liquid states, over varying ranges of temperature between 550" and 1050°K. Stable, mutually consistent, and reproducible electromotive-force data were obtained with most liquid alloys and these are shown in Fig. 1. Investigations were extended below the liquidus tem-

Jan 1, 1967