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By A. S. Koster, G. D. Rieck

X-ray experiments were carried out to show the occurrence of cylindrical texture in drawn tungsten wire. Only a small amount of (110) (110) cylindrical texture could he found in wires of intermediate thickness, i.e., of about 1.5 mm diameter. DRAWN wires of tungsten and other bcc metals like iron and molybdenum show a well-established (110) fiber texture. Now it might be conceivable that in drawing radial stresses remove the randomness of the crystallites around the [110} axis, thus giving a fiber texture of higher symmetry. In the resulting so-called cylindrical textures a specified plane normal coincides with the radius of the wire. Several authors discuss the occurrence of cylindrical textures in bcc metals. ~ieck' found no cylindrical texture in drawn tungsten wires of 165 n diameter. Leber~ states that in tungsten wires of 3 mm diameter a cylindrical {100)(110) texture is developed, which is gradually converted to a normal fiber texture by subsequent drawing. He also reported a definite cylindrical texture at the surface of iron wires. Peck and Thomas3 observed a nonuniform mode of deformation of the grains in transverse sections of heavily drawn tungsten and iron wires. According to Bhandary and cullity4 a swaged iron wire has neither a perfect (110) fiber texture nor a perfect {100}(110) cylindrical texture. It is clear that the concept of cylindrical texture in bcc metals still lacks a firm experimental basis. Leber's eviden~e,~ which seems to be the strongest, rests upon qualitative interpretation of photographs. The appearance of the 110 and 200 lines on the photograph of 3-mm wire, however, can be very well attributed5 to a normal ( 110) fiber texture superimposed on random background; our Fig. 1, giving a Debye-Scherrer diagram of etched tungsten wire of 180 p, is free of cylindrical texture according to all authors, but is quite similar to Leber's diagram. It was therefore decided to use a different method of X-ray texture determination on tungsten wires of diameters where cylindrical textures may be expected.

Jan 1, 1965

By Harold V. Pearce

THE plant of the Boston and Colorado Smelting Company, at Argo, Colo., has not received special notice in technical or scientific publications for some time past. Dr. Peters' described the development of the reverberatory furnace used at Argo, but he dealt almost exclusively with the increase in size and the corresponding gain in capacity. Since the time of his description the changed conditions have led to a modification of the former smelting practice, and this modification forms the basis of the present paper. No claim is made for personal originality in connection with these improvements, in fact, I expressly disclaim any such intention, since nearly every successful step in the development of the process now used at Argo has been suggested by Dr. Richard Pearce at various times during the past 12 years, though perhaps in a different manner of exe¬cution. These changes would undoubtedly have been made before, were it not that many problems of greater metallurgical importance and momentarily of more urgent need thus had to be solved. At the time to which I refer, economic conditions demanded mainly an increase of capacity. Moreover, the determination and placing of exact losses in smelting were not so imperative as they now are. About three years ago, the time of my appointment to the - management of. the works of the Boston and Colorado Smelting Co., the great decline in the price of copper occurred; the Argo plant, in common with all others engaged in the copper-industry, lost heavily in the market-value of the stocks on hand of ore and furnace-products. Added to this was the unfortunate circumstance that the copper-supply of the Argo plant from general sources began to dwindle; in fact, it almost entirely ceased. About this time the smelting-plants in the west-

Mar 1, 1905

By AIME AIME

ANNOUNCEMENT on August 6 of the historic event of dropping an atomic bomb on Hiroshima, Japan, was more dramatic even than V-E day, since that had so long been forecast whereas the bomb production had been the best-kept secret of the war, even though at one time more than 100,000 people had been at work in connection with its production, and some two billion dollars had been spent on the project. Mining men had long been aware of an unexplained abnormal interest in uranium production, and suspected that something of the sort was on foot, while metallurgists were aware that various men of their acquaintance were engaged in some top secret research. The first announcement was soon supplemented by other official releases which told more about the research laboratories for theoretical and pilot studies, and the plants in Tennessee and Washington, but none of them made clear what the modus operandi is of these terrific bombs. Inquiry at Colum. bia University, where Dr. Dunning and his associates had succeeded in 1939 in splitting the uranium atom, and where laboratories known only as SAM have been feverishly active since the beginning of the war, was unproductive, since none of those officially connected with the project could give out anything beyond the official releases.

Jan 1, 1945

By William G. Pariseau

The extraction ratio approach to pillar design in flat seams is based on a mathematically exact analysis that is a reasonable physical approximation to room-and-pillar layouts in many instances. The essentials of the approach are reviewed and then mathematically approximate formulas for pillar design in inclined seams of arbitrary dip are proposed. Detailed numerical analysis of stress about a typical 5 entry, 4 pillar panel at dips of 0, 15, 30, 45, 60, 75 and 90 degrees at low and high extraction ratios show that the proposed inclined seam extraction ratio formulas for pillar normal and shear stresses, although conservative, have an accuracy quite adequate for engineering purposes. Appropriate pillar safety factors for compressive and shear failure and a safety criterion for overturning are specified.

Jan 1, 1982

By A. C. Halferdahl

DURING a study of reactions involving iron sulfides, it became desirable to know approxi-mately the heat of decomposition of pyrite. The values given for the heats of formation of pyrite and ferrous sulfide are 35,500 calories and 23,070 calories respectively. For the reaction 2FeS2= 2FeS+S:, the heat effect would be-24,860 calories. But pyrite gives sulfur and pyrrhotite upon heating and the latter is a solid solution of sulfur in ferrous sulfide. The only meas-urements of this decomposition are those of Allen and Lombard1 of the Geophysical Laboratory who have measured dissociation pressures of both covellite and pyrite and have carefully reviewed the literature. They give a table of values for covellite as determined by Preuner and Brockmoller2 and by Wasjuchnowa3 and compare these values with their own measurements. The conclusion is that the measurements of Preuner and Brockmoller are seriously in error, while Was-juchnowa's values fit in well with those of Allen and Lombard. Wasjuchnowa's measurements were made by a dynamic method, while Allen and Lombard em-plowed a static method on both covellite and pyrite. Tables I and II reproduce the measurements of Wasjuchnowa and of Lombard and Allen on covellite and pyrite.

Jan 11, 1927

By Charles L. Elliot

Worldwide manpower utilization reached a new high at 10,482 professional man-months and expenditures increased to $19.9 million for mining geophysical activity during 1965. This is up from 9323 man-months and $14.5 million in 1964. Worldwide geophysical activity measured in percent distribution of the total manpower utilization and expenditures is presented in the accompanying Figs. 1 and 2. In terms of the total manpower utilization, ground surveys accounted for 61%, airborne surveys 18%, and mining geophysical research activity 21%. For expenditures, the breakdown was ground surveys, 49%; airborne surveys, 3901o; and research, 12%. Industry was responsible in general for 74% of the manpower utilization and 80% of the expenditures. Manpower costs in 1965 averaged $1900 per professional man-month.

Jan 11, 1966

By C. P. Lawhon, J. P. Simpson, W. M. Evans

Data obtained under controlled test conditions using a microbit drilling machine showed that oil emulsified in water muds may either increase or decrease the drilling rate, depending upon drilling conditions. A low-viscosity oil such as diesel fuel can give drilling rates in limestone almost equal to that of water. Data obtained for water emulsified in oil muds showed little decrease in the drilling rate in water-saturated cores as the water percentage of the mud was increased above the 5- to 10-percent range. Changes in drilling rate were found to be dependent upon the oil or water concentration of the mud and upon the type of formation drilled. Changes in static filtration on paper (API filtrate) did not correlate with filtration while the mud was circulated across rock. INTRODUCTION Oil additions to water muds have been reported to increase drilling rates, provide hole stability and improve filtration control. Eckel' showed that water-base emulsion muds used in the West Texas area increased drilling rate with increasing oil concentration up to 15 percent oil by volume, but drilling rate decreased at a concentration of 20 percent by volume. Based on laboratory tests using water muds to drill shale, Cunningham and Goins' reported that drilling rates increased and tendency for the bit to ballup decreased with the addition of oil. Percentage increase in drilling rate varied with the particular formation. They showed oil additions to improve drilling rates ap proximately 75 percent in Vicksburg shale and as much as 150 percent in Miocene shale. Each investigation showed an optimum oil content for the particular formation. Most data that indicated improved filtration control due to oil additions were based on static API Eltrates through paper rather than dynamic filtration through permeable rocks. Some types of dynamic test give a better representation of filtration down-hole while drilling and might be more likely to show some correlation with drilling rate. Static filtration would be important, of course, in relation to hole stability and formation damage. This laboratory's drilling tests, conducted on water-raturated Berea sandstone, indicated that improvements in drilling rate were not evident with increasing oil concentration in water-base muds. Investigation also showed similarity between oil-emulsion (water-in-oil) muds and water-emulsion (oil-in-water) muds while drilling these formations. In Lueders limestone high concentration of water-in-oil muds and high concentration of oil-in-water muds provided the same relative drilling rates. In Berea sandstone there was a large reduction in relative drilling rate with both the oil and water muds that contained low percentages of emulsified fluid. Dynamic filtration rates of water muds on rock did not always decrease with increasing oil percentages even though the static API filtration rates on paper did decrease. Data observed in laboratory drilling of limestone and sandstone indicate that improvements in field drilling operations when water- or oil-emulsion muds are wed may not be the result of increased drilling rates but of improved hole conditions. In some cases, actual drilling rates might be slower but improved hole conditions will result in less total time on the hole. DEFINITIONS Mud pressure—Pressure of drilling fluid as measured after leaving the drilling chamber. This is considered as the approximate mud pressure just past the bit and at the face of the formation. Terrastatic pressure—Pressure representing weight of overburden. Formation pressure—Pressure of formation fluid as measured at outlet of drilling chamber. This is considered as approximate pressure of fluid in the pores of the formation. Differential pressure—Difference between the mud pressure and formation pressure. Relative drilling rate, percent—Drilling rate with experimental fluid divided by drilling rate with water times 100 equals percent. LABORATORY EQUiPMENT AND TESTING PROCEDURES The drilling equipment has been described in previous publications The microbit drill is a closed system (capacity, approximately 7 gal) that can be pressurized to 15.000 psi and heated to 500F. Main components are a drilling chamber, filter-heater, rotary-drive and variable-speed cir-

By E. T. Turkdogan

The activity of sulfur was determined as a function of composition of ferrous sulfide by equilibrating with hydrogen sulfide-hydrogen gas mixtures at 670° , 800°, and 900". The present results supplement the available data over the composition range from 36.6 to 39.5 pct S. The X-ray lattice spacing measurements made are in accord with the available data and indicate that the limiting composition FeSl.008 may be taken for the iron-iron sulfide equilibrium. The growth rate of ferrous sulfide on iron was measured by reacting iron strips or blocks in hydrogen sulfide-hydrogen gas mixtures. Owing to the slow approach to equilibrium between the gas phase and the surface of the sulfide layer, The sulfidation experiments were carried out for several days. It is shown that the growth rate ullimately proceeds in accordance wilh the parabolic rate law. From the parabolic rate constants and the thermodynamic data on iron sulfide the self-difiusivity and chemical diffusivity of iron in ferrous bisulfide are evalualed. The self-diffusivity of iron thus derived zs found to increase with increasing sulfur content. THE ferrous sulfide known as "pyrrhotite" is a non-stoichiometric phase having a wide composition range from about 50 to about 58 or 60 at. pct, depending on the sulfur activity. RosenQvistl studied the thermodynamics of this phase over wide ranges of temperature and composition. Hauffe and Rahmel' and Meussner and ~irchenall~ studied the parabolic rate of sulfidation of iron in sulfur vapor. By using markers, these investigators showed that the iron cations were the predominant diffusing species in iron sulfide. This is confirmed decisively by the self-diffusivity measurements of condit4 who showed that the self-diffusivity of sulfur in ferrous sulfide is several orders of magnitude lower than the self-diffusivity of iron. Although much has been learned from these studies about the Fe-S system, further research on this subject was considered desirable for better understanding of the physical chemistry of iron sulfide. This work was confined to the study of the kinetics of sulfidation of iron in hydrogen sulfide-hydrogen gas mixtures. The results of this study are given in two consecutive parts. Part I, the present paper, is on the parabolic rate of sulfidation of iron and the diffusivity of iron in ferrous sulfide. The second paper, Part 11, is on the kinetics of the surface reaction between hydrogen sulfide and ferrous sulfide. EXPERIMENTAL Three types of experiments were carried out: i) equilibration of ferrous sulfide with gas of known E. T. TURKDOGAN, member AIME, is Manager,Chemical Metallurgy Division, Edgar C. Bain Laboratory for Fundamental Research, U. S. Steel Corp., Research Center, Monroeville, Pa. Manuscript submitted March 6. 1968. ISD sulfur potential; ii) X-ray studies of ferrous sulfide; and iii) measurements of the parabolic rate of sulfidation of iron. Equilibrium Studies. About 1 g of iron powder or foil. contained in a small recrystallized alumina crucible ind suspended from a calibrated silica spring, was reacted with a hydrogen sulfide-hydrogen mixture of known ratio until no further change in weight was observed. %hen the gas composition was changed and the new state of equilibrium was established after several hours of reaction time. The composition of the sulfide was obtained from the initial weight of the sample and the weight after equilibration. X-Ray Studies. The lattice parameters of some of the equilibrated samples were determined using the General Electric XRD-5 diffractometer with a cobalt tube (no filter) set at 40 kv apd 10 ma; the CoK, radiation was taken as 1.79020A. Observed 220 and 311 diffraction peaks of silicon served as an internal comparison standard to correct for possible misalignment of the goniometer. The lattice parameters of the sulfide phase were calculated from the corrected Bragg angles of the 110 and 102 peaks. Rate Studies. In the initial experiments attempts were made to measure the parabolic rate of sulfidation by measuring the gain in weight of a thin iron strip, -0.05 cm thick, suspended from a silica spring in the reacting atmosphere. The preliminary experiments showed that this technique was not reliable for the measurement of the parabolic growth rate of the iron sulfide layer. In the subsequent experiments the data on growth rate were obtained by measuring, on a microscope stage, change in the thickness of the sample after reaction for a specified time in a hydrogen sulfide-hydrogen mixture of known sulfur activity. For each reaction time a new sample was used. Precision-machined iron blocks, 0.5 by 2 by 5 cu cm, were de-greased and annealed in hydrogen for several hours prior to the sulfidation rate measurements. The experiments were carried out at 670°, 800°, and 900°C in gas mixtures having the ratios, and 1.0 for periods of times from a few hours up to 8 days. Apparatus and Materials. A vertical globar tube furnace with a 3-in.-long uniform temperature zone was used. The glass tube fittings were fused on the zircon reaction tube, 1.5 in. diam. The temperature was measured with a Pt-10 pct Rh/Pt thermocouple placed in the hot zone of the furnace inside the reaction tube (an alumina thermocouple sheath was used). A separate thermocouple was used for the temperature controller which maintained the furnace temperature constant within about 2°C. Anhydrous liquid hydrogen sulfide and oxygen-free dry hydrogen from gas tanks were used in preparing the gas mixtures by the constant head capillary flow-meters. In all cases volume flow rate was 1000 cu cm per min at stp, corresponding to a linear velocity of about 6 cm per sec at 800°C; under these conditions

Jan 1, 1969

By W. E. Howlett, R. L. Slobod

Jan 1, 1965

By Donald B. Evans, Robert D. Pehlke

The solubility of nitrogen in liquid Fe-B alloys has been measured up to the solubility limit for the formation of boron nitride. The activity coefficient of nitrogen increases with increasing boron content in the range 0 to 7 wt pct B. From experimen -tal data, values have been calculated for the B-N interaction parameter e3 at temperatures in the range 1550" to 1750°C. A value of 0.038 has been estimated for the boron self-interaction parameter eg at 1550°C. The standard free energy of decomposition of boron nitride into the elements dissolved in liquid iron has been determined to be: ?F° = 45,900 -21.25T in the range from 1550° to 1750°C. The nitride is assumed to be of composition BN. BORON nitride has an unusual combination of properties which make it appear attractive in a wide range of engineering applications. Some of its more important and most recent applications are in the nuclear area, particularly in connection with the liquid-metal cooled reactor concept now receiving considerable emphasis. Boron nitride has a high degree of stability at elevated temperatures. It also has excellent ma-chinability and the ease with which its crystals deform suggests applications as a lubricant. These properties stem from a hexagonal layer-type structure similar to the structure of graphite. One of its primary uses to date has been for seals in liquid-metal pumping systems. It is also used in nuclear reactors as an insulating layer to separate two solid metals which are not themselves compatible under the conditions of temperature and atmosphere in which they are used. Its inertness to liquid metals has also suggested use as a mold-release agent in casting processes. In addition to its excellent machinability and reported inertness to liquid metals such as iron, silicon, aluminum, copper, and zinc, boron nitride has high thermal conductivity and excellent thermal shock resistance. This combination of properties would make it appear ideal as a refractory crucible material for refining of high-purity liquid metals, for example high-quality steels. However, since it is known that concentrations of boron as low as 50 ppm can have a marked effect on the physical properties of certain steels,' in particular on the creep and stress-rupture properties, an investigation was undertaken to define accurately the chemical equilibrium among boron, nitrogen, and liquid iron in the range of steelmaking temperatures. EXPERIMENTAL PROCEDURE Two experimental approaches to this problem were employed: a Sieverts' method and a quenching method. In the first method, the Sieverts' technique was used to measure the equilibrium nitrogen solubility in liquid Fe-B alloys of 0 to 7 pct B as a function of nitrogen gas pressure over the melt. The solubility limit of the boron nitride phase formed was determined by the point of departure of the nitrogen absorption from Sieverts' Law. This technique has been applied to liquid Fe-Ti alloys by Rao and parlee,' to liquid Fe-A1 alloys by Evans and Pehlke,3 and to solid Fe-V alloys by Fountain and Chipman.4 In the second method a melt of liquid iron was held in a crucible of boron nitride under a known partial pressure of nitrogen gas. After thermodynamic equilibrium was attained, the melt was quenched in a stream of helium and then analyzed by wet-chemical methods for boron and nitrogen. The Sieverts' apparatus used in the first method was essentially of the same design as the one described by Pehlke and Elliott.5 The charge materials were vacuum-melted high-purity iron (Ferro-vac E) supplied by the Crucible Steel Co. and -325 mesh boron powder supplied by Cooper Metallurgical Associates of Cleveland, Ohio. The boron contained less than 0.02 wt pct O, according to supplier's analysis. Recrystallized alumina crucibles were used to contain the melt. Examination of solidified melts showed these crucibles to be satisfactory with no evidence of any reaction or physical penetration of the crucible wall by the melt. The melt temperature was measured by a disappearing filament-type optical pyrometer sighted vertically downward on the melt surface through a 1/4-in.-diam sight hole in the crucible lid. The pyrometer was calibrated against the melting point of pure iron in the same apparatus, taking the emissivity of

Jan 1, 1964

By W. C. Leslie, R. M. Fisher, K. G. Carroll

A nitride, believed to be Si3N, has been separated from three nitrided silicon steels. Germanium nitride, Ge3N4, has been prepared from pure germanium. Comparison of the diffraction patterns indicates that the two nitrides are isomorphous; on orthorhombic structure is suggested in place of the rhombohedral structure previously reported for Ge3N4. THE possibility that a nitride of silicon may, under appropriate conditions, precipitate in silicon steels or in steels killed with silicon makes it desirable to have some positive means of identifying such a compound. One such means is the X-ray or electron diffraction pattern of the nitride. A review of the meager data in the literature indicates that the nitride most likely to form is Si3N4, a conclusion supported by the results of a study of nitrided silicon steels to be published shortly by L. S. Darken and R. P. Smith, of this Laboratory. Unfortunately, there is available no diffraction pattern for this nitride. Data have been reported, however, for Ge3N4 which, judging from the similarity between germanium and silicon, might be expected to be isomorphous with Si3N4. An effort was made, therefore, to form such a silicon nitride, to determine its composition and diffraction pattern and, if possible, its structure. To this end a series of three silicon steels was nitrided under controlled conditions with the resultant formation of nitride particles which yielded an electron diffraction pattern in situ. The particles were then extracted from the steel and an attempt was made to determine their chemical composition. X-ray and electron diffraction patterns were also obtained from the extracted particles, which indicate that the nitride is isomorphous with Ge3N4, although a complete determination of the structure has not been possible. These results show that a silicon nitride with a well-defined diffraction pattern can form in silicon steels, and they suggest that this nitride is Si3N4. Materials and Procedures The sillicon steels investigated were In the form of thin sheet or strip and had the composition shown in Table I. The 0.58 and 1.21 pct Si steels were nitrided by holding them at 1110°F in an H2-NH3 atmosphere containing 3 pct ammonia for 48 hr. The nitride particle size was increased by subsequent heating at 1500°F for 13 1/2 hr in helium. The resulting microstructure is shown in Fig. 1. The steel containing 3.20 pct Si was nitrided at 1200°F for 16 1/2 hr after which it was held in helium at 1500°F for 4 hr. Its structure as seen under the electron microscope is illustrated by Fig. 2. As would be expected from the higher silicon content and the shorter holding time at 1500 °F, the nitride particles are smaller and more numerous than those in the 1.21 pct Si steel. The ammonia-hydrogen treatment reduced the carbon content of the steels to a very low level, so no interference was encountered from carbon or carbides. In the case of the 3.2 pct Si steel, the carbon was reduced to 0.003 pct before nitriding by heating in dry hydrogen. Attempts to obtain an X-ray diffraction pattern from polished and etched surfaces of the 1.21 and the 3.20 pct Si steels were unsuccessful. However, an electron diffraction pattern was obtained from the surface of the steels. The interplanar spacings obtained from these patterns arc shown in Table 11, col. 5. The nitride particles were then extracted from all three steels by dissolving the ferrite matrix in bromine-methyl acetate, the solution used in the Beeghly method for the extraction of aluminum nitride from steel. X-ray diffraction patterns of these residues, obtained by means of a spectrometer and by a 57 mm Debye-Scherrer powder camera using filtered cobalt or chromium radiation, are given in Table II along with the pattern obtained by

Jan 1, 1953

By B. F. Tillson

Mining may be defined as a general term for the working of valuable deposits of minerals, either organic or inorganic in origin, for their removal from the crust of the earth. Besides subsurface excavations, mining generically includes opencuts, clay pits and stone quarries, oil wells, sulphur wells, salt wells, placers, coal stripping, and the leaching of ore bodies. The origin of the word "mine" or "mining" is a matter of conjecture. A Celtic origin has been suggested since the Irish word mein, or the mwyn, meant ore, but it seems to have come from an olf French verb mineor, which meant to excavate, to make an underground passage as in the military appraoch to a fortification, sometimes called ?sapping.?

Jan 1, 1949

By Reynold Q. Shotts

CHEMICAL methods, based on the relative rates of oxidation of fusain, bright coal, and dull coal by nitric acid, have been devised to determine these coal components.1-4 Results obtained by oxidation methods for fusain have been checked against results obtained from microscopic methods5, 6on duplicate samples of the same coals, but to the author's knowledge this has not been done for bright and dull coal components. For this reason it is not certain that the two methods of analysis identify essentially the same chemical or physical units. It would be highly desirable to see results of the application of both methods to duplicate samples, but in the absence of any such data the author has attacked the problem indirectly. From the U. S. Bureau of Mines samples were obtained of three Alabama coals which the USBM had analyzed optically and reported on over the past 30 years. These samples were subjected to analyses by oxidation rate methods. Results of this work, and comparisons with the USBM analyses, have been published." This was the first indirect approach to the problem. The present report attempts a second indirect approach by way of internal validation. By nitric oxidation samples of two whole coals were carefully analyzed for fusain, bright coal, and dull coal. One coal was analyzed in duplicate. Duplicate portions of each of the coals were divided into three density fractions by means of heavy liquids. A duplicate portion of one of the coals was divided by sieving into three size fractions. Each fraction was analyzed by oxidation and its percentage composition calculated in terms of fusain, bright coal, and dull coal. Because the weight percent of each fraction was known, a material balance calculation for the whole coal was also made. The resulting reconstituted analysis of the whole coal could be compared to that determined by direct analysis. In addition, specific reaction rate constants were determined for each component and for each whole coal or fraction. Arbitrary reactivity indexes were calculated by dividing by 100 the sum of the products of the percent of each component in the coal and its specific reaction rate constant. The resulting figure was an average reactivity index for each coal or fraction. Weighting the reactivity indexes for each fraction by the percent of the fraction in the coal gave a reactivity index for each whole coal which could be compared to that calculated directly from the whole coal analysis. If oxidation analyses really delineate definite physical entities within the coal, or even definite groups of similar entities, reconstituted analyses calculated from fraction analyses should check closely those made of the whole coal. It probably is true that optical methods identify and describe a greater variety of components than do chemical methods and that variations are wide in the appearance and quantity of those components identified optically. Chemical methods based upon differences in oxidation reaction rates would of necessity be less discriminating, as between similar components, than would optical methods. The procedures followed for oxidizing the samples, analyzing the residues, plotting and calculating the percentage of each component, and calculating its specific reaction rate constant have been fully described.'-' In brief the method originally proposed by Fuchs et al.1 for the determination of fusain consists of the oxidation of small samples of coal in boiling 8N nitric acid in a condenser-fitted flask. After boiling for periods of 1/2 to 4 hr, the unoxidized residue is filtered and washed. The washed residue is treated with normal sodium hydroxide, diluted, and allowed to stand for several hours. The resulting brown liquor is removed, and the filtered residue dried, weighed, ignited, and weighed again. The ash-free residue is expressed as a percent of original dry, ash-free coal. The percent residue is plotted against time, and the extrapolation of this line to zero time gives the percentage of dry ash-free fusain present in the original sample. The shape of the resulting time plots has been explained' by the assumption that they are the result of two different types of reaction, the first part representing a first order reaction with rate a func-

Jan 1, 1956

US underground mine production of nonfuel minerals was 153 million tons of crude ore in 1971, according to a recent US Bureau of Mines report compiled by Dravo Corp. Underground capacity includes all nonfuel mineral commodities and is distributed into three general categories: (1) metallic ores; (2) nonmetallic ores; and (3) construction materials, such as clay, sandstone, and limestone. All three categories are produced by a combination of open-pit and underground methods. While US underground mining represents only 5.9% of total domestic capacity, it is significant in the types of products produced. Domestic supplies of potash, trona, A lead, zinc, sulfur, and fluorspar are almost exclusively recovered from underground mines, as well as a significant portion of the gold, silver, molybdenum, and salt supply.

Jan 7, 1975

By M. J. Marcinkowski, A. Szirmae, R. M. Fisher

Room -temperature hardness measurements obtained from single and polycrystalline samples of a 47.8 at, pet Cr-Fe alloy which were aged for various times al 500°C show a two-fold increase over that of the unaged alloy after annealing for 1000 hr. A detailed examination of the deformation markings in the neighborhood of the hardness imbressions reveals that twinning becomes an increasingly more important mode of deformation as aging proceeds. this observation is shown to be inconsistent with the Proposals that the transformation is eve of order-disorder On the other hand, the results are in agreement with previous observations of Fisher et al. of a coherent chromium-rich precipitate which forms in an iron-rich matrix as a result of a miscibility gap in this alloy system as proposed by Williams . Using the coherent precipitate hypotlzesis as a model, a detailed analysis of the various possible strengthening contributions to both the slip mid twinning stresses is made. In the case of' slip, lattice friction within the chromium-rich phase and the chemical energy associated with the interface between the two phases contribute about 60pet to the total strength. The contributions from coherency strains and modulus differences are thought to contribute the remaining 40 pet of the strength but are difficult to evaluate because of uncertainties regarding the flexibility of the dislocation line. All of the factors have nearly the same or else a smaller effect on the twinning stress in the aged alloy. Twinning is never observed in the unaged alloy because the twinning stress is much higher- than that for slip. With increased aging times, the various contributions to the total stress for both twinning and slip increase, but most of those for slip increase much more rapidly, so that, in the fully aged alloy, it surpasses the stress for twin propagation. When a twin is nucleated by the chance occurrence of an internal stress concentration during a test, the subsequent twin burst results in a low hardness reading. FeRNTIC Fe-Cr alloys from about 15 to 80 at. pet Cr content show considerable change in properties such as hardness, electrical resistivity, saturation magnetization, and so forth, after aging in the vicinity of 500°C.* The most marked change is a large increase in hardness accompanied by a sharp decrease in ductility, so the phenomenon has often been referred to as the 475°C (885°F) em-brittlement problem. Changes in microstructure are rather subtle and most investigators have not been able to observe any X-ray diffraction or metal-lographic changes during aging. There is little doubt that the phenomenon is inherent to the Fe-Cr binary system and is not directly related to the formation of a phase. Two distinct schools of thought have developed during the past decade concerning this problem. Masumoto, Saito, and sugiharal have concluded, from their own specific-heat measurements, that atomic ordering occurs in this temperature range. Pomey and Bastien2 have also attributed the changes in physical properties with aging in the neighborhood of 500°C to atomic ordering. In addition, Takeda and Nagai3 claimed to have found X-ray verification for superlattices corresponding to the compositions FesCr, FeCr, and FeCr3. However, all known attempts to observe superlattices in Fe-Cr alloys using neutron diffraction, which should be much more sensitive, have been unsuccessful. These have been reported by Shull et al.4 for 25 at. pet Cr, williams5 for 75 at. pet Cr, and Tisinai and samans6 for a 28.5 at. pet Cr. steel. The second and more prevalent opinion ascribes the 475°C embrittlement phenomenon to the formation of a coherent precipitate due to the occurrence of a miscibility gap in the Fe-Cr system below about 550°C. This latter concept was first indicated by the results of Fisher, Dulis, and Carroll,7 who were able to extract fine particles about 200Å in diameter from samples of 28.5 at. pet Cr steels aged from 1 to 3 years at 475°C. The extracted material was found to be nonmagnetic, to have a bee structure with a lattice parameter between that of iron and chromium, and to contain about 80 at. pet Cr. Williams and paxton8 and williams5 confirmed these results and first explicitly proposed the existence of a miscibility gap below the a region in the equilibrium diagram. Alloys aged within this gap

Jan 1, 1964

The recent dedication of Magma Copper Co.'s San Manuel, Ariz., electrolytic copper refinery and rod casting plant marks the culmination of a three year, $250 million expansion-modernization program. The new facilities will eventually permit an annual production of 200,000 tons of marketable copper for direct sale to fabricators. The Newmont Mining Corp. subsidiary will produce and market continuous cast 5/16 in. copper redraw rod, full plate cathode copper and sheared cathode plate under its own brand name. Among the four largest in the nation, the new refinery and plant, was built at a cost of $34 million and will be fully automated. In addition, all materials used in the plant will be recycled and no waste, discard or emissions will occur.

Jan 3, 1972

By W. J. Carlson, I. Iwasaki

A previous article reported a combination process for recovering both metallic iron and metallic manganese from the manganiferous iron ores of the Cuyuna Range in Minnesota.' In this process, the iron was recovered by direct reduction and magnetic separation and the manganese was recovered from the nonmagnetic tailing by leaching and electrolysis. The current efficiency during the electrolysis of manganese is quite low, in the range of 60 to 70%, due to the simultaneous plating of hydrogen.2,3 The parameters that affect the current efficiency are (1) the concentrations of the manganese ion and the ammonium sulfate buffer, (2) the effect of autoxidant, (3) temperature, (4) pH, and (5) current density. To study the plating characteristics of manganese metal.

Jan 1, 1969

Sept. 3-8, AIME, Fall Meeting, Industrial Minerals, Minerals Beneficiation, Mining, Geology, & Geophysics, Iron and Steel, and Coal Div., Palmer House, Chicago. Sept. 3-13, AIME, Chicago Section, Centennial of Engineering, Chicago. Sept. 5-8, Engineers' Council for Professional Development, annual meeting, Hotel Sheraton, Chicago. Sept. 11-13, American Institute of Chemical Engineers, Palmer House, Chicago, Ill. Sept. 13, Columbia Section, AIME, Canadian Institute of Mining and Metallurgy, joint all-day meeting, Metaline Falls, Wash. Sept. 18, AIME, Utah Section, Newhouse Hotel, Salt Lake City. Sept. 20, Colorado Section, AIME, Denver. Andrew Fletcher, speaker. Sept. 22-25, American Mining Congress, Metal and Nonmetallic Mining Convention and Exposition, public auditorium, Denver. Sept. 23-25, Institution of Mining and Metallurgy, symposium on mineral dressing, Royal School of Mines. London.

Jan 1, 1952

By Roger K. Clifford, Gary W. Hudiburgh

The amine flotation of feldspar from a magnetite concentrate produced at a domestic concentrator was investigated using zeta potential measurements, Hallimond tube flotation tests, and laboratory-scale flotation tests. The point of zero charge of six feldspars (microcline, orthoclase, albite, anorthite, anorthoclase, and oligoclase) range from pH 1.4 to 2.5. Hallimond tube flotation tests using amine flotation reagents were performed on these feldspars and on gangue material (quartz, albite, and microcline) from the magnetite concentrating plant. Laboratory-scale (623 g and 2500 g) flotation tests were performed on the magnetite concentrate to float the feldspar. The effects of three different collectors, two levels of collector concentration, three pH levels, starch, HF acid and regrind were investigated.

Jan 1, 1977

By D. W. Lillie

Property changes produced by irradiation of Al-0.4 wt pet Li alloys at 270°C to a burnup of 0.155 pct of all atoms are described. Metallographic evidence of the formation of internal pores and the concentration of gases at grain boundaries is shown. Some conclusions are drawn concerning desirable property characteristics for resistance to radiation swelling. RADIATION induced gases are of great practical significance in nuclear engineering since they affect the behavior of fissionable fuels and control rod materials. In fuels the gases xenon and krypton are the major offenders, producing serious em-brittlement at low irradiation temperatures and gross swelling at high irradiation temperatures. In control rod materials containing boron, the production of helium from the B 10 (n, 0) Li7 reaction produces similar reactions. Since the trend in reactor design is for operation at increasingly high temperatures, the phenomenon of high-temperature swelling by these induced gases has been the subject of considerable recent study. The objectives of such work have been to obtain engineering information and quantitative data on the effects in specific fuels and control rods and to obtain further understanding of the mechanism of gas damage so that more intelligent corrective steps can be made. Analogue systems are often useful for the latter objective and in this case alloys containing Li are suitable in view of the reaction Li6 + n - He4 + He 4. Both products are gases and no serious radiation problem is produced to complicate post irradiation handling. Considerable caution is, of course, necessary in any operations in which tritium release is possible. The present program was initiated to provide a detailed study of the effects of He + H3 generated by irradiation in Li-bearing alloys. The results on Mg-Li solid solution alloys have been reported elsewhere.' This paper presents information on irradiation of an A1-0.4 pct Li alloy in which the lithium was present as highly enriched Li6 in order to maximize the radiation burnup. PROCEDURE The original intent in the selection of the alloy content was to have Li in solid solution at all temperatures. It became apparent, however, that the solubility of Li in A1 was substantially lower than that reported in the original reference consulted.' This was substantiated by the work of Nowak3 who reported solubility of less than 0.01 pct Li at 100°C. The alloy used (0.4 pct Li) was therefore two phase at room temperature. The irradiation temperature was estimated to be about 270° C, and at that temperature all or almost all of the Li would be soluble under equilibrium conditions. The precise state of the alloy under irradiation is not known. Aluminum used was 99.996 pct purity (max. impurities Si 0.002 pct, Mg 0.001 pct, Fe 0.0005 pct, and Cu 0.0005 pct). The lithium was obtained from Oak Ridge National Laboratory; 96.1 + 0.1 pct of the lithium was ~i~, but chemical impurities were 0.25 pct Ca, 0.05 pct Fe, 0.02 pct Na, 0.02 pct Cu, 0.01 pct Sr, and 0.01 pct Ba. The two metals were melted in an alumina crucible in a resistance heated furnace in an atmosphere of helium. A l-in. ingot was cast in an iron mold, machined to %-in. round, hot swaged (350°C) to 0.080-in. round, cold swaged to 0.060-in. round, and finally cold drawn to 0.040-in. round. Four-inch wire lengths were then cut and annealed at 250°C for 4 hr in helium. Irradiations were carried out in a VT hole in the Argonne CP-5 reactor. The wires were held in an aluminum jig, sixteen wires per capsule, and were maintained in a helium atmosphere for maximum heat transfer. Eight wires of pure aluminum and eight of Al-Li alloy were placed in each capsule. Argome Laboratory statements were accepted as establishing flux and exposure levels. These were based on previous experience and flux map-

Jan 1, 1961