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By R. P. Walters, M. J. Lynch, D. R. Flinn

The Bureau of Mines evaluated tthhee feasibility of substituting platinum- coated metals for bulk platinum shapes as a means for conserving platinum . Platinum coatings were prepared using four different methods of electrodeposition , then tested and evaluated . In order for platinum coatings to be useful in process environments , they must be thick , adherent , stress - free , and pore - free . The Bureau evaluated direct - current , current reversal , cathode shielding , and pulsed- current plating techniques for producing a pore-free platinum electrodeposit from a molten cyanide bath . Aqueous corrosion tests of Fe - 10Cr substrates coated with approximately 25 μm of platinum showed that pulse plating yielded the most corrosion- resistant and , hence , the most pore -free coatings . The morphology of coating cross sections was in all cases columnar . The average grain size of pulse -plated deposits was independent of thickness , while all other plating techniques produced grains that increased in size as the coatings became thicker . It is believed that the constant grain size in the pulse - plated deposits resulted from better mass transport during the electrodeposition .

Jan 1, 1965

By A. D. McMahon

This survey is one of a series of Bureau of Mines publications designed to serve the needs of Government and industry for comprehensive information on mineral commodities and activities. Copper, a versatile metal, has been vital to all civilizations from prehistoric times to the present. Its essential value in antiquity and until the nineteenth century arose from its malleability and ease of working, its corrosion resistance and durability', its attractive colors in alloyed and unalloyed forms, and, of course, its availability. The principal uses were for tools, utensils, vessels, weapons, pipe, statuary and other objects of art, and for building and architectural pur£~ses where formability, permanence, and beaut)" were necessary qualities. Utilization of copper based on these physical and mechanical properties has grown tremendously for commercial, structural, mechanical, architectural, and art items; and its capacity for forming numerous alloys has led to a myriad of applications from miniature copper and brass eyelets to huge bronze battleship propellers. The early nineteenth century marks the epoch of the greatest use of copper, transmitting electrical energy. This particular property of copper is fundamental to the spectacular growth of the electrical industry and all associated industries relying on electricity for power, light, and heat. More than half of all copper produced is used for transmission of electricity. The copper industry has been able to expand along with the mounting demand because of the ever increasing discovery of resources in the world and advances in mining, metallurgical, and fabricating technologies. World production and consumption rose progressively from about 18,000 tons in 1800 to more than 4.5 million tons in 1960. The estimated world reserve of primary- copper has more than doubled since 1935, being 212 million tons in 1960. Ninety percent of this reserve is credited to eight countries-the United States, Canada, Chile, Peru, the Soviet Union, Poland, Northern Rhodesia, and the Republic of the Congo. The United States share is 32.5 million tons of copper in ore, averaging approximately 0.9 percent. Another reserve being accumulated in the industrial countries of the world is copper products now in use that will eventually be discarded as scrap and become available for recovering secondary copper. In the United States this resource of more than 30 million tons, provides about one-fourth of the annual supply.

Jan 1, 1965

By Wallace W. Key

Mineral raw materials produced in California, other States, and foreign countries were purchased for consumption in quantities valued at over $60 million at 800 of the 1,200 chemical plants operating in California in 1960, according to questionnaires completed by company officials. These and other data received from mineral consumers, producers, dealers, and Government agencies formed the basis for this the first of a series of reports designed to present the intricate features and relationships controlling mineral raw material supply and demand in California industries. The results of this study indicated certain changes in use patterns of minerals in chemica 1 manufacturing; a shift in requirements from metals to nonmeta ls, from inorganics to organics, from natura 1 to synthet ic materia ls , and from distant to local sources of supply.

Jan 1, 1965

By Robert M. Becker

This investigation (in five parts) extends the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The extension of the theory is confirmed by experimental laboratory sampling using standard procedures. The probability distribution functions (the binomial, hypergeometric, multinomial, generalized hypergeometric, and those here called the compound binomial and compound multimomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, and finite population moments are developed from corresponding infinite population moments using a newly defined mathematical operation. The first three experimental moments in laboratory sampling to given weights of particles are compared with the theoretical moments of their corresponding compound mult.inomial distributions. The agreement is striking. The study is divided into five parts. Part 1 deals with probability or random sampling to n items and with all sampling to n items per sample from some one probability distribution. This is the area of sampling covered by well-known theory. Accordingly, the procedures may be different but many of the results are well known.

Dec 1, 1964

By BUREAU OF MINES

Mercury has been used by mankind since prehistoric times. It has been, and is now, widely used in industry and medicine and has unique properties which make direct substitution difficult or impossible. At present its prin- cipal uses are for electrical apparatus, control instruments, electrolytic soda preparation, mildew-proofing paints, pesticides, and medical and dental preparations. Deposits of mercury are less common than those of other base and precious metals, but some of the deposits are very large and have been ample to meet the world's past demands. The price of mercury has had many sharp fluctua- tions, but in general, the limited number of producers has resulted in a more stable price structure than that of many other commodities. The United States has been one of the main producers of mercury, and from 1850 to 1961 produced 3,247,704 flasks. Yearly production since World War II has varied from 4,535 to 38,067 flasks. An estimate of domestic resources of mercury producible at various price ranges was prepared for each mercury mine by combining specific knowledge of mercury mineralization with estimates of potential, based on geologic informa- tion and past production history. The sum of the individual estimates for each price range is shown in a table. A parallel estimate of nationwide production potential was made from a study of past price and production relationships. These were analyzed by plotting yearly production figures against the previous year's price, expressed in dollars of constant purchasing power. An equation was fitted to the data by mathematical means and was used to extend the curve into areas of higher than historic prices. Potential production rates at various price levels were taken from this graph. The estimated yearly production rates were used to make an estimate of total potential based on the premise that produc- tion rates and reserves have a proportionate relationship.

Jul 1, 1964

By John A. Dunn

Continued increase in electric power requirements for mining, brought on by higher capacity mining machines and total mechanization, emphasizes the importance of proper power system design and planning. How effective a mine operates to produce quality coal at low cost depends to a great extent on how well its power system is planned and how well it is maintained. To be planned well it must be adequate to serve all the needs of the mine, it should be safe, there should be a margin for expansion, and it should be easily maintained. In planning a power system for mining coal it is helpful to establish a reliable base for estimating loads. Since most mines are served electric power by utility, power bills for similar mine loads are useful in setting up a base for estimates.

Jan 12, 1964

By Ernst M. Cohn

The demonstrations of the "Silent Sentry" by Union Carbide Corp. in 1957 and of a special tractor-plow by Allis-Chalmers in 1959 ushered in the technology era of fuel cells. The idea for direct conversion of chemical to electrical energy, first published in 1801 by Davy in England and Ritter in Germany, has been kept alive by a few people through 150 years: Grove built the first hydrogen-oxygen fuel cell in 1839; Mond and Langer made electrolyte contributions around 1890 that are still used today; Baur worked on coal-based cells from 1900; Bacon started his work in the '30's, which resulted in the first multi-kilowatt unit in the '50's; Davtyan studied molten-salt electrolytes in the '40's, followed by Ketelaar in the '50's; and Justi developed highly active electrodes in the '50's, to name only some of the pioneers. Despite the tremendous increase in research and development of fuel cells, these direct energy converters are still in their infancy. They will find their functional application in space, where power density must be maximized and product water utilized. These early systems will provide valuable experience in system engineering and reliability.

Jan 9, 1964

By John J. Sense

The Mission unit of the American Smelting and Refining Co., located 20 miles south of Tucson, Ariz., is a high-volume, 15,000 tpd operation which utilizes a relatively light equipment fleet. As such, management is very conscious of the mechanical and operational availability of the equipment in use. One of the key items in attaining this efficiency is a complete and reliable record of mechanical and operational machine availability which is an invaluable guide for: 1) Estimating future equipment and personnel requirements of an operating property. 2) Planning an expansion program of an operating property. 3) Estimating equipment and personnel requirements of a new property. 4) Selection of replacement equipment. 5) Comparison of separate operating properties.

Jan 3, 1964

By A Palynchuk

The development of welded pipe has paralleled the general industrial development and, in particular, that of the petroleum industry. The petroleum industry's need for high-grade, economical pipeline material to make many 'of its projects feasible has been a significant factor in the development of light-wall, high-grade welded pipe. The modern welding processes, such as high-frequency, electric resistance, flash, submerged arc, etc., have some basically different characteristics. The modern high-frequency weld mill is a complex of specialized equipment that is integrated into a production unit. Each component in the unit performs a specific function in the production process. Quality control must be built into the process on an operating basis and, to maintain the quality required for pipeline standards, must be more than a policing operation. The further development of the welded pipe industry will be determined by changing and increasing demands. The technical and economic views and requirements that will influence the development have to be resolved.

Jan 1, 1964

By James J. Scott

Longwall mining has not received a great deal of attention in the United States; however, this system offers many advantages over the conventional room-and-pillar methods now being used. In order to conserve the coal resources of this country, the U. S. Bureau of Mines has investi¬gated the feasibility of adapting European longwall mining methods to American coal seams. Their studies showed longwall mining to be well suited to thinner seams and, greater depths; and, in addition, permitted almost 100 percent recovery of the coal. Most, experiments with this method resulted in higher overall production-costs than were commonly obtained with highly mechanized room-and-pillar techniques This high cost-was largely due to the excessive amount of labor required to maintain adequate roof support with conventional longwall mining techniques. With the substitution of hydraulic-powered, self-advancing roof support systems for conventional supports, this excessive labor cost has been decreased, and longwall mining costs are now competitive with those of modern room-and-pillar mining.

Jan 1, 1964

By Charles A. Stickels, Edward E. Hucke

The dihedral angle, formed by the intersection of three interfaces, is often determined by measuring a sample of apparent angles of intersection seen on a random plane of polish, then comparing the exerimental distribution of angles to the distribution calculated by Harker and Parker. Statistical tests show that the latter distribution does not satisfactorily describe the population from which samples are drawn. It is concluded that the major reason for this discrepancy is the presence of a range of dihedral angles in all specimens. When reasonable care is used experimentally, random measuring error is unimportant. It is shown that measurements made on dispersed second-phase inclusions are subject to a systematic error depending on inclusion size, which can be minimized by using adequate magnification. A dihedral angle, calculated from a sample of observed angles as though a unique dihedral angle were present, is termed an "effective dihedral angle". Experience has shown that "effective dihedral angles'' are reproducible quantities, useful for characterizing samples. Methods of determining an "effective dihedral angle", establishing its reliability, and making comparisons between samples are discussed. THE authors have recently reported measurements of the dihedral angle formed by liquid-lead inclusions lying in nickel grain boundaries.' Di- hedral angles were measured by the statistical method first employed by Harker and parker2 and used subsequently by many other workers.3"8 Since a relatively high degree of accuracy was necessary in the authors' experiments, the reliability of this method of dihedral-angle measurement was examined. Briefly, this method of measuring dihedral angles is usually performed as follows. A multiphase alloy is prepared, equilibrated under conditions which allow sufficient interface mobility to establish equilibrium, quenched to room temperature, then prepared for metallographic examination. A large number of observed angles, formed by the traces of grain boundaries and/or interphase boundaries on the plane of polish, are measured at high magnification. If all orientations of interfaces in the specimen are equally probable, Harker and parker2 showed that the population of observed angles is described by a distribution function containing a single parameter, the dihedral angle, 8. certain properties of the population, e.g., the mode or median, have been calculated from this distribution function in terms of the dihedral angle.3, 9 Thus, if the mode or median of a sample is identified with the corresponding property of the population, a unique value for the dihedral angle is determined. One defect in this procedure lies in identifying the properties of a sample of observed angles with the properties of the population from which they are drawn. If one were to proceed in a more rigorous fashion, it would be necessary to find a function of sample properties which is an estimator of the dihedral angle. Then by determining the distribution function for the estimator one could set limits on the value of the dihedral angle. The most apparent obstacle to this straightforward approach is the complexity of the distribution function assumed to describe the population. In analytical form, the distribution function may be written:2, 10

Jan 1, 1964

By Thomas Pollard

It is truly remarkable how the image of longwall as a method of mining has changed. Between 1920 and 19609 viewed on a world wide basis, longwall was regarded as a' system for difficult and deep conditions and associated with intensive labour extraction. Today the world looks on longwall in the hope that it can produce the next really big break through in productivity, Three correlated machinery developments have made this possible, but it is not only the machinery developments, interesting though these be in themselves, but together with developments in control systems of these machines that longwall now looks so much more attractive, The machinery concerned is, of courses:- 1. The Anderton Shearer Loader - A miner that takes a narrow strip off the, face at rates acceptable to modern mining engineers. 2. An Armoured Flexible, Conveyor which can be kept in close contact with the face and still convey coal as it is snaked over to the faces 3. Powered support systems which can be mechanised and controlled with reliability at any distance from the individual support itself.

Jan 1, 1964

By John Henderson

Densities of melts 0f the lime-iron oxide-silica system in contact with solid iron have been measured by the maximum bubble pressure method in the temperature range 1250° to 1440°C and the composition range 0 to 40 mol pct lime, 15 to 100 mol pct iron oxide, and 0 to 55 mol pct silica. Densities range from 4.65 g cm 3 for wustite at 1440°C to 2.75 g cm-&apos; at 1350°C for a melt containing 30 mol pct lime, 20 mol pct iron oxide, and 50 mol pct silica. The results are interpreted in terms of a postulate that the melts can be regarded as a random array of oxygen ions in which regions of local order exist to satisfy the coordination requirements 0.f the cations. An understanding of the nature of metallurgical slags is basic to the development of a sound theoretical description of heavy metallurgical extractive and refining processes. Because these liquids are complex, direct measurements of their properties has not thrown much light on their structure. This has led to the approach of measuring the properties of simpler liquids, and building up their complexity until slag compositions are reached. In this way the density of liquid iron silicates was measured in a previous study1 and the present work represents a further stage in this synthesis. EXPERIMENTAL The technique used in the measurement of density was the maximum bubble pressure method. Details of the apparatus and procedure were similar to those previously reported,&apos; with the exception that a constant voltage transformer was used to supply the power input to the furnace and six silicon carbide resistance elements were used in place of the molybdenum winding. With these modifications melt temperature could be maintained within 1 centigrade degree during the course of a run. The silica used to prepare the melts was washed natural quartz ignited at 1000°C; wustite was prepared by air-melting A.R. grade ferric oxide in an iron crucible and lime was prepared by air ignition, at 1000°C, of weighed quantities of A.R. grade calcium carbonate, previously air-dried at 110°C. The finely ground constituents were intimately mixed in a glass ball mill prior to melting. Temperatures quoted are accurate to * 5°C and the standard deviation of the density values, calculated by the method of least squares, ranged from 0.5 to 1.8 pet. However, replicate determinations of density on different melts of the same nominal composition at the same nominal temperature did not vary by more than 1 pct, Table I, and this figure has been taken as an estimate of the accuracy of the density results. The density of carbon tetra-chloride was also measured as a check on the absolute performance of the experimental method. At 20°C a value of 1.593 * 0.002 g cm"3 was obtained; this compares with the literature value2 of 1.595 g cm"3. Results of experiments designed to measure the dependence of the density of lime-iron oxide-silica melts, in contact with solid iron, on composition and temperature are shown in Table I. Because iron sometimes precipitated in the sample during quenching, the Fe203 chemical analyses were only poorly reproducible and should be taken as a guide rather than as absolute values. Fig. 1 shows the data from various sources for the density of liquid iron silicates and Fig. 2 shows isodensity contours at 1410°C for lime-iron oxide-silica melts, calculated by graphical interpolation of smoothed curves drawn through the experimental results, together with the 1400°C results of Adachi and ogino3 and Pope1 and Esin.4 Fig. 3 shows the isothermal variation with composition of the volume of melt per gram ion of oxygen at 1410°C and Fig. 4 shows regions in which the temperature coefficient of this volume is negative, positive, or negligible (<0.005 cm3 deg-I). DISCUSSION a) Disparity Between Reported Density Results. Consider the system iron oxide-silica, the results for which are summarized in Fig. 1. Although there is some difference in the temperatures at which the various densities apply, this difference is not sufficiently large to account for the observed discrepancies. The reliability of the present results for the low-silica region has been confirmed by measurement of the density of liquid wustite by three different techniques. At 1410°C the density measured by a balanced-column method was 4.55 g cm"3, by a combination balanced-column and gas-densitometer method 4.59 g emd3, and by a pycnometer method 4.53 g cm"3. Schenck, Frohberg, and Hoffermann&apos; have also reported a value of 4.55 g cm"3 for the density of liquid wustite at 1400°C. It must be concluded, therefore, that neither Pope1

Jan 1, 1964

By Donald C. Strimbeck

The Bureau of Mines, U.S. Department of the Interior, is conducting research and development on a coal-burning gas turbine. This work includes the development of (1) turbine blades resistant to coal ash erosion, (2) equipment to feed coal under pressure to a turbine, (3) an efficient combustion system, and (4) equipment to remove coal ash from the gases that drive the turbine. Initial emphasis is being placed on testing the first turbine ever equipped with blades designed specifically for use with coal as the fuel. Operating tests with this turbine are now in progress. This paper describes the Bureau&apos;s coal-burning gas turbine development program and progress on this operating test.

Jan 1, 1964

According to the principle of similarity, the physical and chemical configurations of a system can be defined by ratios of magnitudes within the system and do not de-pend on the size or nature of units of measurement. In the present work, the similarity principle was utilized in evaluating the reducibility of various iron ores in a rotary batch furnace under optimum operating conditions. It was then used successfully to extrapolate the results, first to the operation of a 20-ft. pilot-plant kiln and then to an industrial-size 80-ft. kiln. By means of this systematic analysis of kiln operation, it was possible to increase the production capacity of the kiln considerably. T HE kilns used by the Strategic-Udy process for the partial reduction of iron ores are, in most aspects, similar to conventional calcining kilns. Iron ore is fed continuously in the upper (feed) end of the kiln and, as the latter rotates

Jan 1, 1964

By Hindmarsh J. W, McCoy A. E R

Instantaneous outbursts of coal and gas have occurred at various times in several working districts of Metropolitan Colliery, N.S.W.They have occurred in headings only, under both hand and mechanised conditions, and with seam gas ranging from mainly methane to nearly pure carbon dioxide. A modification of inducer shotfiring using a shear cut was introduced in 1955, and in 1961 full face firing both to a machine cut shear and off the solid was introduced. The current series of outbursts -1961 to 1963 - has been induced under these systems with full control of the time of outburst, but without prediction, and with some disappointing production features.Various aspects of current conditions and practices at Metropolitan are considered singular, such as the coarse granulometry of outburst coal, the prevalence of floor heave, the absence of strong structures at outburst sites, the possibility of outburst at any stage in pillar formation up to the last few yards, the effect of rate of advance on outburst occurrence, and the mildness of many outbursts experienced.It is concluded that inducer shotfiring is a reliable control but it suffers by comparison with outburst-free conditions, and that control by preyention would be preferable.INTRODUCTIONThe phenomenon of instantaneous outbursts of coal and gas has been described in detail previously (Hargraves, 1958). Briefly, it is a combined gas and stress hazard of deep coal mining, usually occurring in virgin work and during active face advance, when coal and seam gas burst from the face into the workings.Instantaneous outbursts have occurred sporadically at Metropolitan Colliery, N.S.W., since 1895. Early outbursts were recorded as firedamp and recent outbursts are of blackdamp.Mining methods used have been conventional hand work, with progressive and relatively complete mechanisation over the past 25 years to substantially conventional...

Jan 1, 1964

By J. McCreedy

The Ontario Division of The International Nickel Company of Canada, Limited, operates five underground mines and one open pit on the rim of the Sudbury Basin located in the Province of Ontario, 230 miles northwest of Toronto. Four of the mines, Frood-Stobie, Creighton, Murray and Garson, lie on the South range of the Basin within a 10-mile radius of the City of Sudbury; the fifth mine, Levack, is on the North range, about 30 miles northwest of the city. The ores are mined primarily for nickel and copper, the principal minerals being pentlandite and chalcopyrite. Other elements recovered from the ores in varying quantities are platinum, palladium, ruthenium, iridium, rhodium, cobalt, selenium, tellurium, iron, sulphur, gold and silver. In 1962, the total underground ore production was over 10,800,000 tons which was mined mainly by blasthole and caving methods with the remainder by cut-and-fill, square set, and undercut-and-fill techniques.

Jan 1, 1964

By J. Wade Watkins

One potential peaceful application of nuclear explosives is stimulating the production of liquid or gaseous hydrocarbons from essentially nonproductive deposits of petroleum, natural gas, oil shale, and tar sands. Within the United States the appreciable difference between producible proved reserves and ultimate reserves and resources of hydrocarbon deposits is of such magnitude that much petroleum, natural gas, shale oil, and bitumen will not be produced unless significant technological progress is made in production techniques. The shattering effect of contained nuclear explosives and, to a lesser extent, the heat produced, have been considered as stimulative forces when the thickness, depth, and nature of such deposits permit considering the use of nuclear devices. Mechanical production problems would be less in an oil or gas reservoir than in an oil-shale or tar-sands deposit. Also, tar-sands resources in the United States may not be adequate to warrant serious consideration of applying nuclear-explosives stimulation. Gas reservoirs should present the least- radioactive-contamination problem. The technical feasibility of using nuclear explosives cannot be evaluated fully at present. Additional information is needed on the effects of pressure, heat, and radioactivity on the solids and fluids of hydrocarbon deposits, the nature and extent of induced fractures in different rock media, and the possibility of isolating and confining or removing radioactive contaminants. Final technical feasibility can only be determined by a field test. If technical feasibility is established, economic feasibility will depend upon the comparative cost of producing hydrocarbons by nuclear explosives and by conventional means. It is probable that an economic comparison would favor nuclear stimulation only where devices of relatively high yield could be used practicably and safely.

Jan 1, 1964

By R H. Hallam

The Mattagami mining district encompasses a favour-?able belt of folded Keewatin-type rocks, with intercalated sediments and intrusives of late Keewatin age. This environment has been subjected to periods of basic and acidic intrusion. The orebodies lie within the fold structure and are associated with faulting and shearing of considerable magnitude. The No. 1 orebody contains 60 to 70 per cent massive sulphides. The minerals, in their order of abundance, are generally: pyrite, sphalerite, pyrrhotite, magnetite and chalcopyrite. It is evident that the broad geological structure of the district is amenable to ore deposition. There are two ? prominent linear expressions which comprise this broad structure. Both strike directions lie at the edge of, or are related to, a complex gabbro-anorthosite-peridotite zone. The fact that eleven of the ore zones discovered to date coincide with the broad structure indicates its over-all importance. It is estimated that the production from Mattagami Lake Mines will be in the range of 600 to 700 tons of zinc concentrate and 70 tons of copper concentrate per day.

Jan 1, 1964

By Takashi Katsura, Avnulf Muan

Equilibrium relations in the system FeO-Fe2O3 Cr2O3 have been determined at 1300°C at oxygen pressures ranging from that of air (0.21 atm) to 1.5 x 10-11 atm. The following oxide phases have stable equilibrium existence under these conditions : a sesquioxide solid solution with corundum-type structure (approximate composition Fe2O3-Cr2O3); a ternary solid solution with spinel-type structure (approximate composition FeO Fe2O3-FeO Cr2O3) and a ternary wüstite solid solution with periclase-type structure and compositions approaching FeO. The metal phase occurring in equilibrium with oxide phase(s) at the lowest oxygen pressures used in the present investigation is almost pure iron. The extent of solid-solution areas and the location of oxygen isobars have been determined. ThE system Fe-Cr-O has attracted a great deal of interest among metallurgists as well as ceramists and geochemists. Metallurgists have studied the system because of its importance in deoxidation equilibria, ceramists because of its importance in basic brick technology, and geochemists because of its importance for an understanding of natural chromite deposits. Chen and chipman1 investigated the Cr-O equilibrium in liquid iron at 1595°C in atmospheres of known oxygen pressures (controlled H2O/H2 ratios). The main purpose of their work was to determine the stability range of the iron-chromite phase. Hilty et al.2 studied oxide phases in equilibrium with liquid Fe-Cr alloys at 1550°, 1600°, and 1650°C. They reported the existence of two previously unknown oxide phases, one a distorted spinel with composition intermediate between FeO Cr203 and Cr3O4, the other Cr3O4 with tetragonal structure. They also sketched diagrams showing the inferred liqui-dus surface and the inferred 1600°C isothermal section for the system Fe-Cr-O. Koch et al3 studied oxide inclusions in Fe-Cr alloys and also observed the distorted spinel phase reported by Hilty et al. Richards and white4 as well as Woodhouse and White5 investigated spinel-sesquioxide equilibria in the system Fe-Cr-O in air in the temperature range of 1420" to 1650°C, and Muan and Somiya6 delineated approximate phase relations in the system in air from 1400" to 2050°C. The present study was carried out at a constant temperature of 1300° C and at oxygen pressures ranging from 0.21 atm (air) to 1.5 x 10-11 atm. The chosen temperature is high enough to permit equilibrium to be attained within a reasonable period of time within most composition areas of the system, and still low enough to permit use of experimental methods which give highly accurate and reliable results. These methods are described in detail in the following. I) EXPERIMENTAL METHODS 1) General Procedures. Two different experimental methods were used in the present investigation: quenching and thermogravimetry. In the quenching method, oxide samples were heated at chosen temperature and chosen oxygen pressure until equilibrium was attained among gas and condensed phases. The samples were then quenched rapidly to room temperature and the phases present determined by X-ray and microscopic examination. Total compositions were determined by chemical analysis after quenching. In the thermogravimetric method, pellets of oxide mixtures were suspended by a thin platinum wire from one beam of an analytical balance, and the weight changes were recorded as a function of oxygen pressure at constant temperature. The data thus obtained were used to locate oxygen isobars. The courses of the latter curves reflect changes in phase assemblages and serve to supplement the observations made by the quenching technique. 2) Materials. Analytical-grade Fe2O3 and Cr2O3 were used as starting materials. Each oxide was first heated separately in air at 1000°C for several hours. Mixtures of desired ratios of the two oxides were then prepared. Each mixture was finely ground and mixed, and heated at 1250" to 1300°C in air for 2 hr, ground and mixed again and heated at the same temperature for 5 to 24 hr, depending on the Cr2O3 content of the mixture. A homogeneous sesquioxide solid solution between the two end members resulted from this treatment. A Part of some of the sesquioxide samples thus prepared was heated for 2 to 3 hr at 1300°C and oxygen pressures of 10-7 or 1.5 x 10-11 atm. Reduced samples (either iron chromite

Jan 1, 1964