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Large deposits of manganiferous iron ores, representing several million tons of metallic manganese, occur in the United States. The Minnesota deposits of such ore are of outstanding importance because of their size, state of development, ease of mining and proximity to the Great Lakes, which permits water transportation to steel centers. In view of the fact that our steel industry requires large quantities of manganese, for which no satisfactory substitute has been found, and because our reserves of ferro-grade ore are comparatively small, the development of methods that will make our large deposits of manganiferous iron ores available as a source of ferromanganese is an important problem. Realizing the importance of this problem, some years ago the North Central Station of the U. S. Bureau of Mines and the Minnesota School of Mines Experiment Station undertook jointly the development of methods for recovering the .manganese content of manganiferous iron ores in a form suitable for the production of ferromanganese, the 80 per cent. alloy indispensable in producing steel. Two types of manganiferous iron ores have been described in previous reports.' The brown ores are higher in iron and lower in manganese than the black ores; the black ores are more siliceous but contain less phosphorus. The utilization of the iron content of the brown ores in the production of steel appears to furnish the best basis for their treatment. The method of attack has been to work out modifications in iron and steel practice so as to recover manganese in the form of slag comparable to ferro-grade ores. The greater part of the experimental work has been conducted with a 6-ton blast furnace and a 1/2-ton basic open hearth. This paper is devoted mainly to open-hearth tests in which high-phosphorus spiegel

Jan 1, 1930

By J. O. Marsden

Part I in this series of papers considered the chemistry of medium-temperature pressure leaching of copper sulfide concentrates and reviewed the metallurgical testing and initial process development for this technology. This initial work resulted in the development of a process flowsheet utilizing superfine grinding (to a P98 of 12 to 15 µm and P80 of 6 to 7 µm), pressure leaching at 160° to 170ºC, followed by conventional solution extraction (SX) and electrowinning (EW) for the recovery of copper. However, this process required a significant amount of concentrated acid to be fed to the pressure leach vessel to meet the reaction requirements, representing a cost of between $0.03 and 0.05/lb copper (2006 basis) produced by the process. It was immediately recognized that the development of a process that did not require such a large acid addition would be advantageous. This paper, which is Part II in the series, describes the development of a process that incorporates medium-temperature pressure leaching and direct electrowinning (DEW) in a novel and innovative process flowsheet. Phelps Dodge (a subsidiary of Freeport-McMoRan Copper & Gold Inc.) refers to this as the ?MT-DEW-SX? process. Part III in this series covers the large-scale demonstration of the MT-DEW-SX process at Bagdad, Arizona; and Part IV addresses the development and design of a full-scale commercial application at Morenci, Arizona.

Jan 1, 2007

By B. T. Brady

Recent theoretical, experimental, and field studies conducted by the Bureau of Mines suggest that rock failures may be predicted and, in some instances, controlled. Theoretical studies that were later corroborated by laboratory and field studies predict that a seismic anomaly will precede rock bursts and/or roof falls in mines. The seismic anomaly is predicted to consist of an increase in the number of seismic events occurring in the immediate vicinity where the failure 1s nucleated. This increase will then be followed by a dramatic decrease of seismicity in a broad region that surrounds the location of the impending failure. The dimensions of this region allow a preliminary estimate of the time to failure (measured from the time the seismicity increase began) as well as an estimate of the energy that will be released at the instant of failure. Field observations indicating that this predicted behavior does precede rock bursts and a roof fall are presented in this report. Implications of results to the problem of failure control in mines that experience massive rock failures are discussed.

Jan 1, 1978

By W. M. Dressel

This Bureau of Mines report describes a shaft closure demonstration project in which 11 inverted pyramid-shaped plugs were used to plug abandoned open mine shafts in Galena, KS, The inverted pyramid-shaped forms, fabricated from steelplate, were designed so that the inverted base would be larger, by 4 ft on a side, than the approximate size of the shaft opening at the surface residuum-solid rock interface. After the surface openings of the shafts were trimmed with a backhoe, the steel forms, complete with reinforcing, were lowered into the openings and filled with concrete; the remaining portions of the openings above the plugs were backfilled to slightly above the surrounding surface level with waste rock and soil. Location and elevation monuments were installed for long-tern evaluation of the success of the project.

Jan 1, 1985

By Dan Brown

This paper presents a case study of a cyclic lateral pile load testing program performed on two 18-in square prestressed concrete piles (PSC) in Savannah, Georgia. The load test program was developed to simulate the lateral behavior of a single pile under seismic loading conditions for the design and construction of a large LNG storage tank. The lateral load tests included cyclic loading to measure possible degradation in soil response followed by static loading to large displacements (around 6 inches at the loading point). The lateral load was applied through a reciprocating jack positioned to push and pull the piles against each other. The test piles were instrumented with multiple displacement transducers, downhole inclinometer, and strain gauges. This paper provides an interpretation of the test results regarding the pile performance and soil response to monotonic and cyclic lateral loading. A backfitted computational model of the soil resistance was developed to match the test results using the LPILE computer program. The load-deflection and deflection/moment versus depth comparisons suggest that this model appears to capture the behavior relatively well within the general range of suitability for design purposes. New design curves were developed based on the soil parameters derived from the lateral load test results.

Jan 1, 2003

By L. Flett, S. Woods, C. Deredin

"Following a significant reduction in world Imperial Smelting Furnace (ISF) capacity from 2003 to 2008, a major optimization initiative was successfully carried out on the lead upgrading and bulk (zinclead) flotation circuits in the Brunswick Concentrator.This paper describes the process improvements that have taken place in order to reduce the quantity of bulk concentrate:•,Increase in lead upgrading rougher flotation circuit capacity•,Installation of a closed-circuit bulk regrind utilizing MillPebs and 150 mm Cavex hydrocyclones•,Installation of two additional cleaner flotation stages on the bulk circuit•,Optimization of the manipulated variables in the lead upgrading and bulk circuitsINTRODUCTIONThe Brunswick Mine (Xstrata Zinc Canada) is located near Bathurst, New Brunswick and is one of the world’s largest lead/zinc mines. Milling of ore commenced in 1964 from the No. 12 orebody, with an expansion in 1966 to accommodate ore from the No. 6 open pit mine. The planned closure of the mine will take place at the end of the first quarter in 2013. The ore is a complex massive sulphide, consisting of approximately 20% valuable minerals, 60% pyrite and 20% silicates.A simplified flowsheet for the concentrator is given in Figure 1. The overall flowsheet involves SAG milling, secondary ball milling, selective flotation, and dewatering by thickening, filtering and drying. The complexity of the flowsheet evolves from the requirements for fine grinding and the production of four concentrates: zinc (sphalerite), lead (galena), copper (chalcopyrite) and bulk (sphalerite plus galena).Primary hydrocyclone overflow feeds the copper-lead aerator-roughers for flotation at pH 9.0 with soda ash. Plant xanthate (80-20 sodium isopropyl and potassium amyl) and AP407 are used as collectors in the copper-lead circuit. The rougher concentrate is directed to the copper-lead regrind circuit and the tailings are fed to the secondary grinding circuit. The secondary hydrocyclone overflow from the secondary grinding circuit feeds the copper-lead rougher-scavenger banks. Rougher concentrates are reground to a P80 of 28 µm prior to three stages of copper-lead cleaning. The first stage of cleaning is done in an open circuit with the tail reporting to the cleaner scavenger. The cleaner scavenger concentrate reports to the regrind circuit and the cleaner scavenger tail combines with the rougher/scavenger tail to feed the zinc circuit. The second and third stages of cleaning are performed in closed circuit with the cleaner tail being recycled to the copper-lead regrind circuit. The average final concentrate grades 23% Pb, 3% Cu and 704 g/t Ag, and is fed to the copper separation circuit."

Jan 1, 2013

By John R. Reynolds

This paper describes mining and milling methods of the American Smelting & Refining Co. at the Morning mine in the Mullan area of the Coeur d'Alene mining region in Idaho and is one of a series of Bureau of Mines reports dealing with methods and costs of mining throughout the United States. The Morning mine has been described previously in a Bureau of Mines report published in 1930,2/ and the milling methods and costs at the Morning concentrator were presented in a Bureau of Mines report published in 1932. 3/ These reports are supplemented by this publication, which presents data to show the effect of changing times and conditions on a typical medium-size mining operation during the latter part of its history, when costs were rising and production was from increasingly greater depths. The report contrasts two periods in the history of the mine-periods not too far separated in years but considerably different in economic conditions. During the first period (1939) costs of labor and materials were moderate, mining operations were just being transferred from the main shaft to deeper workings opened from the offset shaft, and the operation prospered. During the second period (12 years later) production costs had increased following the national trend in all industry, mining was from greater depths near the bottom of the ore body, and the operation was becoming unprofitable. Mining on the lower levels of the property ceased in 1953.

Jan 1, 1956

By John D. Spencer

Surveys to establish the quantity and quality of coals available for metallurgical, industrial, and energy use, investigations to develop better mining methods, and studies aimed at improving the health and safety of those who mine the coal highlighted Bureau of Mines research and technologic work on coal in 1968. Also being developed are more efficient methods of coal preparation, transportation, storage, and utilization. Supplementing this effort are projects designed to assure minimum disturbance of land, water, and air resources. Research centers and laboratories of the Bureau of Mines are listed in appendix A. Publications released during 1968 are cited with the various projects and in appendix C. Organizations that cooperated in the work in various ways are cited in appendix B.

Jan 1, 1969

By R B. Stewart

Where pasture production is the intended land use of the areas to be reclaimed, the creation of a suitable growing +medium is a major objective. To achieve this land reclaimers require a sound understanding of the proposed mining plan and a knowledge of the physical, biological and chemical properties of materials intended for resurfacing disturbed areas. Where the original soil is not being replaced in its natural state, research is usually required to determine an alternative growing medium. Results from field research conducted on waste material from the Waihi Gold mine are reported with emphasis on the significance of soil depth in relation to pasture production in this environment.  Problems in extrapolating field research to large scale operations are also considered.   Essentially the requirements for successful pasture production, on surrogate growing medium, are akin to conventional approaches used in New Zealand in the development of unimproved agricultural land. High inputs of fertiliser are initially needed, especially where volcanic soil is used, and careful management of pastures and soils is required to minimise soil erosion and create a sustainable system. In the first three to five years of pasture production, grazing use of the land requires to be dictated by pasture availability and soil conditions and not by animal feed requirements. The use of light stock (young dairy or sheep) is recommended.   Successful land restoration requires a team approach by a range of cooperative specialists including engineers, soil scientists, farm managers, agricultural contractors, landscape architects and environmental officers.

Jan 1, 1991

By Charles Knilans, Tassos Grammatikopoulos, Nicole Hoffmann

"Twin Metals Minnesota LLC, (TMM) has recently completed a prefeasibility study evaluating the development and operation of an underground copper (Cu), nickel (Ni), platinum (Pt), palladium (Pd), and gold (Au) mining project on the Maturi deposit in northeastern Minnesota.The Maturi deposit is a magmatic Cu-Ni-sulphide deposit occurring along the basal contact of the South Kawishiwi intrusion, comprised of heterogeneous troctolites to gabbros forming a tabular body designated the BMZ (basal mineralized zone). These rocks provide the major gangue mineralogy (plagioclase, olivine, and clinopyroxene) with local, minor rock-forming orthopyroxene, biotite, magnetite, and ilmenite. Altered silicates exist within local fracture and/or alteration zones, which are commonly associated with minor faults in the regional area. The Maturi deposit is comprised of four main mineralized zones within the BMZ, referred to as Stage 1, Stage 2 (S2), Stage 3 (S3), and Upper Heterogeneous. Chalcopyrite, cubanite, pentlandite, and pyrrhotite are mainly hosted within the S2 and S3 units, with talnakhite frequently occurring within the S3 unit.A cross-discipline approach combining geology, geochemistry, metallurgy, QEMSCAN™ mineralogy, and mine planning has been implemented to develop a preliminary geometallurgical model and life of mine metallurgical performance forecast. This paper provides an overview of the methods that were used to develop the model and forecast, and discusses the advantages of such a model in project development and evaluation.INTRODUCTIONThe TMM Project proposes mining a copper-nickel-palladium-platinum-gold-silver (Cu-Ni-PGM) magmatic sulphide deposit situated in the Duluth Complex of northeastern Minnesota, USA. The prefeasibility study proposes a 45,000 million tonnes per day mine and concentrator facility to produce two saleable concentrates. The mine will access two separate deposits, Maturi and Maturi Southwest. Saleable concentrates are the final products of the sequential flotation plant where a high grade Cu concentrate is produced followed by a Ni concentrate."

Jan 1, 2015

By Bradford F. Townsend, Colin R. Speers

INTRODUCTION This is the first in a series of papers addressing practical tunnel lining design. The format for this and future papers is to present a particular topic and support the presentation of the guidelines by the practical application of a case history. The primary intent is to provide guidelines for the geotechnical and structural design of tunnels where the tunnel size and/or ground conditions dictates that systematic support of the excavation is required following each increment of excavation. This method of tunneling is commonly referred to as Sequential Excavation and Support(SES) and is also commonly termed the New Austrian Tunneling Method (NATM) The authors developed the design guidelines from experience gained over the past two decades during the design and construction of several major railway, highway and water-transfer tunnel projects in Africa and Asia. During this time it has been possible to compare the performance of the as-constructed structures to the predicted performance as given by the design process. Excavation was typically carried out in widely varying ground conditions (weak-bedded rock, jointed hard rock, and soil-like poorly cemented rock with groundwater). It is therefore intended that the design guidelines could be applied, in general terms at least, to any tunnel excavated in any ground mass condition with any ground material type (hard rock, soft rock, bedded rock, soft ground, and soil) with or without ground water. This first paper is an introductory paper that defines the scope and a brief outline of the design issues that may be presented in detail in later papers. What is design? It may be thought of as any rational/verifiable/justifiable process whereby a concept is transformed into information that can be used to bring the concept to reality. In the case of a civil structure, design may be defined as that process, which is documented and can be audited, that determines information such as the shape (form) of the structure, the dimensions (size) of the structure, the thickness and strength of structural members that comprise the structure, etc. This information can be used to compute the time, money and resources required for

Jan 1, 2005

By Verya Nasri

This paper presents analysis of damages and rehabilitation design for three major French rail-way tunnels built in mid-19th century. The La Nerthe tunnel underwent ovalization deformation with excessive displacement at the springline, and pinching and bursting of the liner bricks at the crown due to tectonic residual stresses with very high lateral earth pressure. The Saint-Louis les Aygalades tunnel invert was subjected to undulatory deformation resulting in tracks misalignment, which was caused by non-homogeneity of mechanical and hydraulic properties of the ground. The Roches de Condrieu tunnel required widening to comply with the increase in dynamic envelope of trains due to their larger cross section and higher speed. The applied rehabilitation methods and constraints of work in these busy mainline railway tunnels have been discussed in detail.

Jan 1, 2008

By N. C. Dunham

"The Bureau of Mines exploratory work on the Bear Lodge, Wyo., fluorite property wider the strategic minerals Program was completed in November 1944. Exploration consisted of surface trenching, shaft sinking, and drifting at shallow depth. Doak C. Cox of the Federal Geological Survey visited the area during the latter part of 1944 and napped the Bear Lodge property.The Bear Lodge property is situated in the Black Hilts National Forest in eastern Crook County, Wyo., 6 miles north of the community of Sundance (fig. 1). Sundance is 29 miles northwest of Upton, Wyo., a station on the Chicago, Burlington, & Quincy Railroad and 43 miles southwest of a siding on the Chicago & Northwestern Railroad, 3 miles south of Belle Fourche, S. Dak. U. S. Highway 14 passes through Sundance in an east-west direction. Sundance may be reached from the south over U. S. Highway 85 and Wyoming State Highway 585.The Bear Lodge property i a situated in the Boer Lodge Mountains in secs. 15, 22, and 23, T. 52 N., R. 63W., 6th P.M.The topography in the vicinity of the fluorite deposits consists essentially of rounded hills which slope gently to the valley floors. Near the north end of the Property the terrain steepens locally, and the canyon walls are Precipitous along the courses of several streams. There is an adequate supply of water and native timber for mining purposes. The average elevation near the deposits is 5,700 feet.The climate of the region is relatively moderate. The summers are usually warm, with frequent rainstorms. Temperatures often fall below zero during the winter months. Snowfalls are moderate to heavy.Fluorite occurrences in the Bear Lodge area have been known since 1914; however, fluorite was not discovered on the Bear Lodge property until 1943, when prospectors working on a nearby manganese deposit found fluorite mineralization in the limestone. No production has been recorded from the property."

Apr 1, 1946

Eco-Efficient Gravity Separation Solutions in India Sustainable development and social responsibility issues are a principal aspect of mineral processing operations around the world. With the need for more environmentally effective technologies, some gravity separation systems have provided eco-efficient mineral processing solutions in places where it is not otherwise viable because of lack of fresh water or for other environmental reasons. Advanced spiral separation technologies developed in Australia offer a cost effective and environmentally viable way to process minerals. In particular, we review recent case studies of spiral plants commissioned in India where environmentally sustainable solutions to design problems included the use of spirals operated with sea water and the use of high capacity (HC) spirals to provide low consumption of energy and materials and a reduced plant footprint. This paper evaluates the performance of various spiral plants in India and how critical environmental issues which affect the overall viability of wet concentrating processes where resolved.

Sep 13, 2010

By Steve Stuart

Deep-sea mineral SMS deposits present some of the world’s most challenging conditions for drilling equipment. As robotic seabed drilling services mature so too the ways that clients engage with service providers to maximise their data requirements. This presentation reviews key considerations for planning and executing a successful seabeddrilling program in variable mineralised deposits. Some of the means of collaboration between robotic seabed drilling contractors and those hiring their services are explored; where improved efficiencies and recoveries over the period of a drilling programme could be achieved. Potentially new technology or methodology can be looked at to further improve these approaches.

Sep 1, 2014

By Malcolm Scoble, Jean-Marc Robert, Luciano Piciacchia

"An approach to the in situ testing of mine backfills is outlined. It has been developed to provide a measure of the effective strength and stiffness of such materials after placement in stopes. This paper is based upon recent field studies undertaken at five Quebec mines. Details of the selected instrumentation, supporting equipment and testing procedures are reviewed. The mechanical behaviour of the backfills is reported and related to their physical properties. This approach represents an economical, simple and reliable means to assess the mechanical characteristics of backfill materials as an aid to both mine design and placement quality control. IntroductionDevelopments in backfill and mining method technology are creating a pressing need to develop effective techniques for characterizing the physical and mechanical properties of backfill in situ, rather than relying on traditional laboratory testing. The development of bulk mining methods is creating the requirement to more fully understand the nature of exposed fill faces to design for stability in pillar recovery operations. Other backfill technological developments currently receiving widespread attention are high density placement and the use of alternative additives to Portland cement. In Canada, U.S.A. and South Africa attention is also being placed on employing backfill to alleviate rockburst hazards(1,2.3l. In situ testing offers the potential to measure the geomechanical properties of backfill once placed in stopes , in order to assess its actual role in pillar recovery and ground support. Similarly, it offers the ability to provide some quality control during backfill placement. This role is seen as becoming increasingly important with the growing recognition of the need to pay greater attention to the mode of placement, which governs segregation and variation in the properties actually achieved by the backfill after placement."

Jan 1, 1987

By Thomas M. Barczak

Advancements in support technology have occurred to a large extent because of the demands of the mine operators. Shield supports are no exception. The most notable changes in shield technology in the past decade have been increases in shield capacity and life expectancy, which have increased by a factor of 4 and 7 respectively since the inception of the shield support 25 years ago. The purpose of this paper is to set goals for the future generations of longwall shields. These goals include: (1) 100,000 cycle life expectancy, (2) improved hydraulic diagnostic capability, (3) smart load control with adjustable setting pressure algorithms, (4) composite material design to reduce weight and increase shield width, (5) constant set leg cylinder design, (6) improved joint design to reduce wear and stress, (7) advancements in leg cylinder socket design, and (8) an instrumented shield to measure in-service structural component loading. These design issues will continue to push the envelope in longwall shield technology that has provided the safest and most productive mining system employed in the history of mining. In preparation for this, a historical examination of shield failures is made and recent trends in shield design are evaluated. Design practices to improve structural margins of current designs are also addressed.

"The Pierre Beauchemin Mine attained commercial production in January 1989, and went on to produce 23 968 ounces of gold for the year, 3% higher than forecast. Underground development was accelerated to prepare the way for the production of an estimated 40 000 ounces in 1989.IntroductionThe Pierre Beauchemin Mine is located nine miles west of the city of Rouyn-Noranda (Fig. I).As a result of the amalgamation with Sullivan Mines in October 1987, the mine is now entirely owned by Cambior Inc.The Eldrich deposit was discovered in 1953and began production in 1955, closing in 1962 following the decrease in gold prices and the simultaneous decrease in silica content in the ore, which was sold to the Noranda smelter for flux. A total of 717 000 tons grading 0.14 oz Au/t were produced during this period.From July 1984 to October 1987, an underground exploration program was carried out by Sullivan on the Eldrich mining concession and the nearby Flavel property. The first phase of the program included reinstallation of surface facilities and dewatering of the Eldrich Mine. Following the completion of the first phase, extensive exploration was carried out, including a major program of diamond drilling. It was then decided to deepen the shaft to a depth of 1800 ft to access a new zone called the No.5 Zone .Following the amalgamation with Sullivan in October 1987, Cambior assumed the role of operator for the project, and continued the shaft deepening work that had already been started. A feasibility study was completed in April 1988 and the Cambior board of directors approved a production decision for the Eldrich-Flavel project.The preproduction program extended from May to December 1988 and was aimed at preparing the stopes in the upper part of the mine and at developing the mine infrastructure at the bottom of the mine.The mine was officially opened in August 1988. Cambior renamed the project the Pierre Beauchemin Mine in recognition of Pierre Beauchemin's pioneer-work."

Jan 1, 1990

By Cássio Barbosa

O desenvolvimento da indústria metal-mecânica nos últimos anos tem levado à demanda de materiais com propriedades mecânicas e de resistência à corrosão cada vez melhores, com o objetivo de suportar severas condições de uso e assim garantir melhor desempenho para equipamentos e estruturas que utilizam os componentes fabricados com estes materiais. Neste contexto, é de fundamental importância conhecer bem a microestrutura destes materiais, que influencia consideravelmente suas propriedades. O propósito deste trabalho é realizar uma caracterização preliminar de ligas não ferrosas (de alumínio e de cobre) utilizadas na fabricação de componentes antifricção. Com esta finalidade, técnicas como microscopia ótica, microscopia eletrônica de varredura (MEV), envolvendo análises de EDS e de EBSD, assim como ensaios de microdureza foram utilizadas para caracterizar a microestrutura do material (liga Cu-Sn-Bi). Os resultados obtidos neste estudo permitiram a identificação das fases presentes neste material.

Aug 16, 2017

By H. W. Knott, M. H. Mueller

The crystal structures of Ti2Cu, Ti2Ni, Ti4Ni2O, and Ti4Cu20 have been determined using powder specimens examined by X-ray and neutron diffraction. Lattice constants have been determined for all four phases using X-ray powder diffraction films. Atom positional parameters of all four phases have been determined from observed neutron intensities. X-ray diffraction calculated intensity data have been presented also for the phase Ti2Cu to point out the particular suitability of neutron diffraction in this case. Interatomic distances have been determined using the positional parameters obtained from neutron diffraction. ALTHOUGH some investigations of the crystal structures have been made of these four compounds previously,'-13 it was the purpose of the present investigation to expand the previous work in order to locate the various atoms, determine their coordinates, and to confirm or to correct some of the previous work. It was convenient to group these four compounds together since they are related chemicallv and/or structurally. The compound Ti2Cu is tetragonil; and Ti2Ni, Ti4Ni2O, and Ti4CU2O are all large fees of the same space group. Ti2Cu has been previously reported as a fee phase by Laves and Wallbaum;1 and Rostoker2 which was possibly the oxide phase, Ti4Cu20. Joukainen, Grant, and Floe;3 and Trzebiatowski, Berak, and Ramotow-ski4 have also reported a phase of this composition. karlsson5 has reported a small fct phase of the composition Ti3Cu which may be the presently discussed Ti2Cu phase. More recently Ence and Margolin6 have reported a small fct phase for Ti2Cu and the present authors7 together with Nevitt8 have briefly reported it to be a bet related to the fct with a co three times the length of the co of the fct and have also reported that this phase has a very limited composition. Further refinements will be reported which have varied some of the parameters of this bct structure slightly. Ti2Ni has been reported as a fee phase by Laves and wallbaum;1 Duwez and taylor;9 Rostoker;2 Poole and Hume-Rothery;10 and Yurko, Barton, and parr.11 In a later paper Yurko, Barton, and parr12 have given the complete structure of this phase based on an X-ray diffraction study which was independently confirmed with neutron diffraction by Mueller and knott.7 Additional crystal structure information will be given. Ti4Ti2O, Ti4Cu2O, and a number of other compounds including Ti4Fe2O have been reported as fcc phases by Rostoker,2 and more recently Nevitt13 has confirmed the Ti4Ti2O phase. Rostoker,2 however has reported diffraction lines for Ti4Fe2O which do not have all odd or all even indices. These lines, therefore, cannot be observed if this compound has a fee structure. This same error has crept into the diffraction results reported for TiNi2O and Ti4Cu20 in the ASTM powder data which has been credited from Rostoker's data. Complete crystal structures of these two phases will be presented. Although all four of these structures have large unit cells and hence do not lend themselves for completely resolved neutron powder patterns, a sufficient number of individual reflections was observed for solving the structure. They also serve as good examples of some of the advantages to be gained by using both neutron and X-ray diffraction techniques. EXPERIMENTAL PROCEDURE All of the alloys were prepared by arc melting. The starting metals had the following purity: Cu 99.999 pct, Ni 99.83 pct, and Ti 99.92 pct. Oxygen was introduced into the two oxide phases as chemically pure TiO2, with the remainder of the titanium coming from the above mentioned metal. All of the sample buttons were annealed in evacuated Vycor tubes, the two binary phases for 5 days at 700°C and the two oxide phases for 3 days at 900°C. Oxygen analyses were performed on all four phases by two independent laboratories with the following amounts of oxygen present in atomic percent; Ti2Cu-0.06, Ti2Ni-1.03, Ti4Ni2O-13.95, and Ti4Cu20-13.87. The stoichiometric amount for the oxide phases is 14.29 at. pct. Since all of the samples were very brittle they were easily reduced to a powder for diffraction measurements. The lattice constants given in Table I were determined for the four compounds from X-ray diffraction patterns of powder samples exposed to filtered copper radiation using a 114.59 mm diam Debye-Scherrer type camera using the Straumanis loading. None of the patterns showed a detectable amount of a second phase. The lattice constants were obtained from an IBM 704 computer program employing a least squares treatment with systematic correction terms as previously reported.14

Jan 1, 1963