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US 4,183,899 - Flow process for chlorinating ilmenite. A laminar flow of a mixture of ore, a carbonaceous reductant, and chlorine gas or other chlorinating agent is passed through a reaction zone maintained at a temperature of 1350 to 1950°C and a product stream Including titanium tetrachloride is withdrawn from the zone. The atomic ratio of carbon to oxygen in the feed mixture is greater than 1:1, and the molar ratio of chlorine to titanium solids In the product stream is between about 0 5.1 and 2:l. Titanium chlorides and metallic iron are recovered separately from the product stream. J.P. Bonsack, assigned to SCM Corp, Jan. 15, 1980 21 pp. (423-79). Filed. 3-10-78 (885,442).

Jan 1, 1982

By Aureal T. Cross

THIS paper is a review of the published literature on research in coal geology, principally exclusive of resource studies, which appeared or became available during 1950 and the latter part of 1949. This report is not to be construed as being complete. The papers referred to in the bibliography are those among many more, which were read either in full or in abstract. Undoubtedly other papers were published which either escaped the author's notice or were not available to him. Those which were seen in abstract only (about one fourth of those listed) were not available in time for the inclusion of more than a notice. An outline of all papers listed in the bibliography has been arranged by subjects and reasonable subdivisions with some papers cited under more than one subject. Most papers are indexed according to the principal subject of discussion or research only as to an unusual or noteworthy section of the entire report. There will likely be some disagreement as to the quality or merit of some of the papers selected and the specialist may be supercritical of the outline or organization of papers in his field. It may be that attention has occasionally been drawn to papers reporting old information or conclusions of questionable value. Conferences and Meetings One of the best indications of the growing interest in coal geology problems in the United States is the increasing number of times this field has been the focus of attention at conferences and meetings. Notable among these are the joint meeting of the Society of Economic Geologists and the Geological Society of America at El Paso, November 1949, at which the principal thesis was concerned with low rank carbonaceous fuel deposits, especially of western United States. Among the papers given which are already available were those presented by Barghoorn,'" Parry? Roe? and Parks."' At the annual meeting of the Botanical Society of America in New York, December 1949, a joint meeting of the Paleobotanical and Microbiological Sections was held for which a symposium on Microbiology in Relation to the Geologic Accumulation of Organic Complexes was organized. Publication of the six papers presented by Ralph G. H. Siu, Elso S. Barghoorn, Irving Breger, Claude E. ZoBell, James M. Schopf, and A. C. Thayson is anticipated. At the regular meetings of the Paleobotanical Section at the same time, several other papers of interest reported on coal ball studies, partial coalification of petrified wood, and floras. In Chicago, April 1950, a symposium on Applied Paleobotany was held by the Society of Economic Paleontologists and Mineralogists in conjunction with the American Association of Petroleum Geologists. The five papers presented at this meeting dealt with the use of Paleozoic plant microfossils for stratigraphic work, J. M. Schopf, Devonian-Missis-sippian fossils of the black shales, Aureal T. Cross, Mesozoic plants of stratigraphic value, Th. Just, plant microfossils of the Tertiary, L. R. Wilson, and studies of the Brandon lignite, Elso S. Barghoorn. Early publication of these in the Journal of Paleontology is expected. The Nova Scotia Research Foundation and the Nova Scotia Dept. of Mines sponsored an excellent 3-day conference in June 1950, which dealt with several aspects of coal geology. Papers on coal classification, P. A. Hacquenbard, structure and sedimentation problems in Nova Scotia, T. B. Haites, new techniques of thermal analysis, W. L. White-head, geochemical investigations of Nova Scotia coals, Irving Breger, the role of fossil plant spores in coal correlation and the stratigraphy of the coal-bearing strata of the Appalachian Region, Aureal T. Cross, were given. Some discussions of these papers by those in attendance were recorded, and the entire proceedings is being prepared for publication. In September 1950, an unusual 3-day field conference was held by the Ohio and West Virginia Geological Surveys under the sponsorship of the Coal Geology Committee. This study of the stratigraphy, sedimentation, and nomenclature of the Upper Pennsylvanian and Permian coal-bearing strata of southeastern Ohio, southwestern Pennsylvania, and northern West Virginia was augmented by two discussions on associated rocks (clays and shales) and stratigraphic nomenclature at Wheeling and Morgantown, West Va. An extensive guidebook was prepared, and transcriptions of the Morgantown meeting were made. As a follow-up of the September field conference, a round-table discussion was held on this general topic at a special open meeting of the Coal Research Committee in conjunction with the November meeting of the Geological Society in Washington. Short prepared statements to invite discussion were given on each of several topics by L. M. Cline, Carl 0.

Jan 1, 1953

By Aureal T. Cross

THIS paper is a review of the published literature on research in coal geology, principally exclusive of resource studies, which appeared or became available during 1950 and the latter part of 1949. This report is not to be construed as being complete. The papers referred to in the bibliography are those among many more, which were read either in full or in abstract. Undoubtedly other papers were published which either escaped the author's notice or were not available to him. Those which were seen in abstract only (about one fourth of those listed) were not available in time for the inclusion of more than a notice. An outline of all papers listed in the bibliography has been arranged by subjects and reasonable subdivisions with some papers cited under more than one subject. Most papers are indexed according to the principal subject of discussion or research only as to an unusual or noteworthy section of the entire report. There will likely be some disagreement as to the quality or merit of some of the papers selected and the specialist may be supercritical of the outline or organization of papers in his field. It may be that attention has occasionally been drawn to papers reporting old information or conclusions of questionable value. Conferences and Meetings One of the best indications of the growing interest in coal geology problems in the United States is the increasing number of times this field has been the focus of attention at conferences and meetings. Notable among these are the joint meeting of the Society of Economic Geologists and the Geological Society of America at El Paso, November 1949, at which the principal thesis was concerned with low rank carbonaceous fuel deposits, especially of western United States. Among the papers given which are already available were those presented by Barghoorn,'" Parry? Roe? and Parks."' At the annual meeting of the Botanical Society of America in New York, December 1949, a joint meeting of the Paleobotanical and Microbiological Sections was held for which a symposium on Microbiology in Relation to the Geologic Accumulation of Organic Complexes was organized. Publication of the six papers presented by Ralph G. H. Siu, Elso S. Barghoorn, Irving Breger, Claude E. ZoBell, James M. Schopf, and A. C. Thayson is anticipated. At the regular meetings of the Paleobotanical Section at the same time, several other papers of interest reported on coal ball studies, partial coalification of petrified wood, and floras. In Chicago, April 1950, a symposium on Applied Paleobotany was held by the Society of Economic Paleontologists and Mineralogists in conjunction with the American Association of Petroleum Geologists. The five papers presented at this meeting dealt with the use of Paleozoic plant microfossils for stratigraphic work, J. M. Schopf, Devonian-Missis-sippian fossils of the black shales, Aureal T. Cross, Mesozoic plants of stratigraphic value, Th. Just, plant microfossils of the Tertiary, L. R. Wilson, and studies of the Brandon lignite, Elso S. Barghoorn. Early publication of these in the Journal of Paleontology is expected. The Nova Scotia Research Foundation and the Nova Scotia Dept. of Mines sponsored an excellent 3-day conference in June 1950, which dealt with several aspects of coal geology. Papers on coal classification, P. A. Hacquenbard, structure and sedimentation problems in Nova Scotia, T. B. Haites, new techniques of thermal analysis, W. L. White-head, geochemical investigations of Nova Scotia coals, Irving Breger, the role of fossil plant spores in coal correlation and the stratigraphy of the coal-bearing strata of the Appalachian Region, Aureal T. Cross, were given. Some discussions of these papers by those in attendance were recorded, and the entire proceedings is being prepared for publication. In September 1950, an unusual 3-day field conference was held by the Ohio and West Virginia Geological Surveys under the sponsorship of the Coal Geology Committee. This study of the stratigraphy, sedimentation, and nomenclature of the Upper Pennsylvanian and Permian coal-bearing strata of southeastern Ohio, southwestern Pennsylvania, and northern West Virginia was augmented by two discussions on associated rocks (clays and shales) and stratigraphic nomenclature at Wheeling and Morgantown, West Va. An extensive guidebook was prepared, and transcriptions of the Morgantown meeting were made. As a follow-up of the September field conference, a round-table discussion was held on this general topic at a special open meeting of the Coal Research Committee in conjunction with the November meeting of the Geological Society in Washington. Short prepared statements to invite discussion were given on each of several topics by L. M. Cline, Carl 0.

Jan 1, 1953

By P. G. Shewmon, H. E. Collins

A study has been made to determine the sites at which sulfur adsorption occurs on copper surfaces. measurements were made of the relative torques, Ys, at the intersection of twin boundaries with surfaces near the three low-index orientations, i.e., (100), @lo), and 011), over a range of H2S/H2 ratios. HZS concerztvations j'ro~n 3 to 1500pp)n between 830" and 1050°C were used. It is concluded that sulfur adsorption occurved preferentially though not exclusively at edge sites near the (100) and (110) surfaces in the HzS range — 700 Ppm giving rise to negative torques near these orientations. Beyond this HzS range, adsorption occurred at all sites. Near the (111) surface, 7/y little with HzS concentration up to approxiwzately 75pptn. Above this range, the results indicate adsorption is occurring OH both terrace and edge sites. SCIENTIFIC interest in surfaces and their interactions with a gaseous environment dates back to the beginning of the 19th century. The scientific luminaries of that period—Faraday, Maxwell, Rayleigh, Dewar, and Gibbs—were already concerned about such processes. However, it has only been within the past several decades that adsorption on metal surfaces has been actively studied. This increased interest in adsorption has been brought about by the advent of new and improved experimental techniques and apparatus, e.g., ultrahigh vacuum, and field-emission and ion microscopes. However, most of the work done using these techniques has been carried out at low temperatures. When adsorption studies have been made at either low or high temperatures, they usually gave no indication of the particular surface orientations or type of sites on which adsorption was occurring. In the last few years, there have been a series of studies in which the surface tension, y,, and/or its derivative with respect to orientation, 7, have been studied as a function of orientation and atmosphere.'-7 Nearly all of the work on the relative torque,* ~/y, silver annealed in hydrogen and air.6 Recently Winterbottom and Gjostein" have used a modified and more accurate Mykurian method to determine the y plot of gold in hydrogen The only work in which T/~, has been measured over a range of chemical potentials for a given solute, p2, is that of Robertson and shewmon7 on the Cu-0 system. They measured T/Y, vs Po, (10"" to 10- l3 atm) at 1000°C in various mixtures of Hz0 and HZ. From this work they estimated the value of p2 at which one half of the surface sites are occupied with oxygen, pg, as being in the range 10- l6 to 10- l5 atm of oxygen. They also found that increasing Pa increased the magnitude of ~/y, near the (111) and (100) orientations. This indicates that oxygen is not adsorbed preferentially at step edges, but uniformly over all surface sites. In addition, they did one experiment on sulfur adsorption on copper surfaces, which indicated that sulfur adsorption decreases ~/y, near the (100) orientation, while not affecting ~/y, near the (111). This could be interpreted as indicating that sulfur adsorbs preferentially at step edges near the (100). In this paper the primary objective of the work has been to carry out a study of sulfur adsorption on copper surfaces over a range of temperatures and p,. In conjunction with this work, thermal grooving at grain boundaries has been examined as a method of determining the effect of sulfur adsorption on y,. METHODS Ideally, one would like to have information on the quantity of solute adsorbed on a surface and the types of sites at which it is absorbed as a function of p2. The total quantity adsorbed or the surface excess is given by the thermodynamic equation Thus data on the variation of y, with pz indicates the value of p2 at which adsorption becomes appreciable and the quantity adsorbed. The type of adsorption site is more difficult to deduce but information on this can be obtained from the variation of rz with 8, the angular deviation of the surface orientation. This is obtained from the thermodynamic equationlg Data on t and ys as functions of p2 have been obtained by the following methods. 1) Twin Boundary Grooving—By determining the effect of adsorption on the torque, 7, where T is the variation of surface energy, y,, with orientation, it is possible to obtain some indication as to the preferred sites of adsorption. Experimentally, the torque value measured is the relative torque, 7/ys The twin boundary grooving technique suggested by Mykura'' was used in this study to determine near the three low-index orientations— (loo), (110), and (111). Mykura's equation relates 7 /yS to measurements of the di-

Jan 1, 1967

Truman H. Aldrich W. Lawrence Austin W. S. Ayres John Henry Banks Andrew A Blair Walter M. Brodie R. C. Canby

Jan 1, 1932

By Yves Dardel

INTRODUCTION SINCE the first determination of Dumas1 in 1880, many authors have tried to measure the solubility of hydrogen in solid aluminum, or at least the amount of dissolved gas in it. However, the interpretation of the results which have been obtained is still difficult. Sieverts,2 then Baukloh and Oesterlen,3 during their gassing experiments could not determine any solubility of hydrogen in solid aluminum. On the other hand, Portevin, Chaudron and Moreau,4 leaving the determination of the hydrogen solubility beyond the scope of their experiments, measured only the amount of gas that they could extract by high voltage positive ion bombardment and found up to 151 cm3 of gas per 100 g of metal. Winterhager,5 by repeated vacuum extraction during severe cold rolling, extracted up to 161 cm3 per 100 g. In both series of experiments, the extracted gas contained chiefly hydrogen with a small amount of nitrogen, carbon monoxide, carbon dioxide and methan. Later, Schmidt and von Schweinitz6 as well as Chaudron and Moreau7 showed the importance of the adsorbed layer of hydrogen, the extracted quantities being proportional to the surface and not to the weight of the sample, when its cleaning was not perfect. In earlier experiments, Steinhauser8 extracted from more massive samples nothing but a little amount (< 0. 5 cm3 per 100 g) of hydrogen, carbon monoxide and methane. Thus, according to these experiments the quantity of dissolved gas is probably very small and the effect of the surface could falsify the results of the extraction. However, owing to the care taken by Chaudron and his coworkers, it was clear that all the hydrogen extracted could not come from the superficial layer, or that the links which bound hydrogen to the surface were so strong that the usual method of cleaning could not destroy them. After the main parts of the experiments reported here had already been carried out, Eborall and Ransley9 published the results which they obtained with an analysor having an accuracy of 0.03 cm3 per 100 g, while that of the usual apparatus was only about 0.2 cm3 per 100 g. During all their experiments the adsorbed layer would have been a difficulty, for the value of the adsorbed hydrogen was approximately equal to that of the dissolved amount. [ ] Since always keeping the same adsorbed layer is very difficult, an error in the correction for the adsorption can be made when using the apparatus of Eborall and Ransley, as well as the earlier apparatus,

Jan 1, 1948

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

Executive A. R. LEDOUX, Chairman GEORGE D. BARRON SIDNEY J. JENNINGS J. V. N. DORR J. E. JOHNSON, JR.¬ Membership J. E. JOHNSON, JR., Chairman KARL EILERS F. F. SHARPLESS R. M. RAYMOND LEWIS W. FRANCIS Finance J. V. N. DORR, Chairman CHARLES F. RAND J. V. W. REYNDERS Library E. GYBBON SPILSBURY,&apos; Chairman ALEXANDER C. HUMPHREYS GEORGE C. STONE&apos; JOHN H. JANEWAY BRADLEY STOUGHTON Papers and Publications BRADLEY STOUGHTON, Chairman

Jan 1, 1923

By R. F. Hehemann, S. T. Zegler

The w phase in zirconium alloys containing more than G pct Nb can form in a difjUsionless manner during quenching or with composition change during aging at temperatures below 550°C. The latter treatment establishes a metastable equilibrium between an w phase containing 5 pct Nb and a ß phase containing 45 pct Nb. The superconducting transition temperat~ire of quenched Z?-10 pct Nb and Zr-15 pct Nb alloys is increased by aging at 375°C and both alloys exhibit the same Tc after prolonged aging. The superconducting transition both in the quenched and in the aged alloys is relatively sharp (occurring ovev a temperature range of <0.5°K), and is interpreted in terms of the microstructure that characterizes the ß-w) mixture and proximity effects postulated for thin-film superconductors. At elevated temperatures alloys of the transition elements from groups 4 to 6 in the periodic table exhibit wide ranges of mutual solubility in the bcc structure. Except for compositions that are high in a group 4 element? the bcc structure can be retained at room temperature by quenching and several systematic studies of the influence of composition on superconductivity in bcc alloys have been reported.&apos;&apos;2 The high-temperature bcc form (ß) of the group 4 elements—titanium, zirconium, hafnium—is not retained upon quenching but instead transforms marten-sitically to the hcp structure (a). The Ms temperature can be lowered by alloying the group 4 metals with a solute from a higher group and with a critical amount of solute the martensitic transformation can be suppressed. The 3 phase, however, is not retained without modification. Rather, a metastable phase, w (in particular in titanium- and zirconium-base alloys), occurs over a fairly wide range of compositions above that required for suppression of the martensitic transformation.3,4 As in the formation of a, the transformation of ß to w occurs in a diffusionless manner during quenching and the temperature for its initiation (ws) is lowered by increasing solute content. The ws temperature can be well below room temperature and reversibility of the transformation allows w that forms on cooling to low temperatures to disappear again when the sample is returned to room temperature.5 In Zr-Nb alloys the w phase can also be formed during aging at temperatures below 550°c.5 In this treatment, a metastable equilibrium is established between a niobium-rich ß phase and a zirconium-rich w phase. The present study of Zr-Nb alloys was undertaken to examine the influence of microstructure: as controlled by composition and heat treatment, on the superconducting transition temperature, Tc. MATERIALS AND PROCEDURE The alloys were prepared from zirconium crystal bar that was spectrochemically pure except for 30 ppm of Al, 40 ppm of Cu, 100 ppm of Fe, and 1 ppm of each B and Pb. The niobium used was 99.5+ pct pure containing according to the suppliers&apos; (Stauffer Chemical Co.) analysis a maximum of 50 ppmO, 60 ppm of N, 30 ppm of C, 5 ppm of H, 200 ppm of Ta, 50 ppm of Mo, and 15 ppm each of Fe, Co, and Ni. The alloys were prepared in the form of buttons weighing approximately 4 g by arc melting on a water-cooled copper hearth in an inert-gas atmosphere. All alloys were heat-treated in the ß-phase region for 3 days at 1000°C and water-quenched. For heat treatment, the specimens, 0.5 cm in diam by 1.0 cm long, were wrapped in zirconium foil and sealed in an inert-gas atmosphere inside quartz capsules. Quenching was done by breaking the capsules under water. Subsequent aging treatments of Zr-10 pct Nb and Zr-15 pct Nb alloys were done by placing the specimens in a lead bath at 375°C and quenching in chilled brine. The phases present in the quenched and aged alloys were identified by optical and X-ray metallography. X-ray powder patterns were taken at room temperature with a 114.6-mm-diam Debye-Scherrer camera and CuK-a radiation. Superconducting transition temperatures were determined from magnetic-permeability measurements6 in a 10 oe field. The superconducting transition temperature was determined from a plot of galvanometric deflection as a function of temperature by extrapolation of the linear portion of the curve to zero deflection. In Figs. 1 and 3 the arrows indicate the temperature range of the transitions. RESULTS AND DISCUSSION Superconductivity in Quenched Alloys. In Fig. 1 Tc for alloys quenched from 1000°C is plotted against nominal composition. Indicated also in Fig. 1 are results of metallographic studies. Alloys containing less than 5 pct Nb transform martensitically to a during quenching from 1000°C and Fig. 1 demonstrates that Tc increases significantly as the niobium concentration in a is increased. On the basis of the Bardeen-Cooper-Schreiffer theory of superconductivity7 it seems most likely that this increase in Tc results from an increase in the density of electronic states as zirconium is alloyed with niobium. This increased density of states has been revealed clearly in low-temperature specific-heat measurements.8 The martensitic transformation to a is suppressed when the alloy content exceeds 5 pct Nb. In the range from approximately 6 to 30 pct Nb, quenched alloys consist of a mixture of B and w phases and the amount

Jan 1, 1967

By AIME AIME

A PAPER prepared by James A. Adams, development engineer of the fitline & Smelter Supply Co., and presented at the last Annual Meeting of the A.I.M.E. in New York City, de- scribed a new automatic pulp density controller which has had a most favorable reception. Manual control has until now been the universal practice in spite of its shortcomings; samples of pulp for density determination were often improperly taken, and only at the operator&apos;s convenience, so that the trend in density changes was frequently missed, and the grinding circuit al- lowed to operate under something less than the most efficient conditions.

Jan 1, 1940

By I. Zaplatynskyj, G. C. Kuczynski

SINCE the excellent studies of metal powder compaction executed by Kamm, Steinberg, and Wulff, no work on the subject has appeared in the technical literature. Kamm et al. were the first to investigate quantitatively the distribution of density in a powder compact, as a function of pressure, height and diameter of the die, powder particle size, etc. For this purpose they devised a very ingenious method. They inserted a thin lead grid into a die and then filled the die with powder. During cold pressing, the lead grid -moved downward. Due to its deformability it followed closely the downward descent of the adjacent powder. The die was then radiographed and, from the deformations of the grid openings measured on the radiographs, the density in the vicinity of each opening was evaluated. Their findings led them to the conclusion that the friction on the side walls of the die is a major controlling factor of the density distribution inside the cold pressed powder compacts. However, it is difficult to conduct tests similar to those of Kamm, Steinberg, and Wulff in a processing plant laboratory, which usually lacks the necessary expensive radiographic equipment. The purpose of this note is to describe a method which makes it possible to determine the density distribution in green powder compacts with the same accuracy as the lead-grid method but which is far simpler and faster and requires only standard laboratory equipment. Instead of using a lead grid, the hardness at selected points of the sectioned compact is determined. If the relationship between hardness and density is known the density distribution is readily obtained. This relationship is easily found from measuring hardness and densities of thin compacts. In such compacts the density, for all practical purposes, is constant throughout. The method was tested on a Plast nickel powder, grade FlA-A20, kindly supplied by Plast Metals Co. Thin compacts (height to diameter ratio 0.2) were pressed in a single action cylindrica1 die at various pressures. The density of the compacts was determined by weighing and by measuring the height and diameter with a micrometer. Subsequently the Rh hardness was determined. Up to ten readings were taken on each specimen. The difference in hardness readings on each compact was never greater than three corresponding to about 0.1 g per cu cm uncertainty in density. By varying the compaction pressure of the samples, a whole scale of densities was obtained allowing construction of a set of density-hardness calibration curves. To test the method several compacts of different height were pressed under varying pressures. Die walls were always well lubricated. After pressing, the compacts were mounted in bakelite and halved by grinding, and hardness readings taken along the diameters of the specimens. The distance between adjacent indentations was about 2.5 mm. After hardness readings were translated into densities, contour maps of densities of the compacts were prepared. One of them is reproduced in Fig. 1. The areas encompassed by the curves are labeled with numbers representing the density in g per cu cm of those regions. In Fig. 2 the same results are re-plotted to emphasize the radial density changes at various depths. The results thus obtained confirm the findings of Kamm, Steinberg, and Wulff kentioned previously. They are recapitulated here briefly. 1—The densest part of a compact pressed from one side is at the outer circumference at the top and the least dense part at the bottom, at the outer circumference. Figs. 1 and 2 show this clearly. 2—The density near the cylindrical surfaces of the compact decreases uniformly with height from top to bottom. 3—The density variation increases with the height to diameter ratio. References R. Kamm, M. A. Steinberg, and J. Wulff: Trans. AIME (1941) 171,&apos;R. p. 439 ;MetaLs Technology (February 1941). R.p. Kamm, M. A. Steinberg, and J. Wulff: Trans. AlME (1949) 180, 2R.P. 694; MetalS Technology (December 1948).

Jan 1, 1957

By AIME AIME

M ODERN metallurgy properly belongs to this century. The great advance made in this science is directly attributable to the discovery of the Roentgen rays. Application of the results of this discovery, together with the more recent corroborating studies in electronic diffraction have definitely and for all time established this science. Metallurgists today speak with familiarity of the atoms of the different metals in terms of their orientation, atomic volumes, lattice structures, dimensional lattice constants distance of nearest approach, and the like. One matter of profound interest, which is quite staggering to the imagination of the human mind, is the enormity of the number of atoms even in a small particle of metal. As an illustration, let us compute the number of atoms in the volume of one cubic centimeter in a single grain of absolutely pure copper. Eighteen and a fraction cubic centimeters equal the volume of one cubic inch.

Jan 1, 1940

By E. Posnjak

IT is rather the general belief that acidified solutions of ferrous salts are readily oxidized when in contact with air, and often elaborate pre-cautions are taken to prevent it. This, however, is not the case and several statements may be found in the literature expressing surprise at the extreme slowness with which oxidation takes place when air or oxygen is bubbled through such a solution. Thus C. Baskerville and R. Stevenson1 "observed with surprise" that no. oxidation apparently took place, as shown by titration with 0.5 N KMnO4, when a stream of air was passed for 3 hr. through an acidified solution of ferrous ammonium sulfate or ferrous sulfate. The same authors state that even the presence of salts such as cobalt, chromium, copper, manganese, etc., which usually act as oxygen carriers, had "no effect upon the oxidation as was observed by, passing air for 3 hr. through solutions of Mohr&apos;s salt acidified with sulfuric acid." While this statement will be proved further on to be at least partly incorrect the slowness of the oxidation of ferrous salts alone has been previously established by McBain.2. His investigation also showed that the rate of oxidation increases markedly with an increase in the concentration of ferrous sulfate as well as that of oxygen; the concentration of free acid had a comparatively small influence, which in the case of sulfuric acid was to retard slightly the rate of reaction. More recently R. Thomas and E. T. Williams3 investigated the catalytic effect of nitric oxide on the oxidation of ferrous salts, which had been earlier patented by McCulloch.4 They found that the probable mechanism of the catalytic action was the oscillation of the catalyst between two stages of oxidation and its interaction alternately with the oxygen and the ferrous iron.

Jan 1, 1927

By A. H. Geisler, J. H. Keeler

Preferred orientations in unalloyed zirconium were determined by the Geiger-counter spectrometer X-ray diffraction technique. With increasing P-annealing temperature the following textures were obtained: l—a retained a-annealing texture, 2—additional orientations predictable from the a-p (Burgers) relationship, and 3—a texture derived from a cube texture in the p phase. Earlier work on cold-worked and a-annealed zirconium was reappraised to show a quantitative dependence of rotations on temperature and to identify spurious areas of some of the pole figures. IN a previous paper,&apos; the preferred orientations of high purity zirconium sheet were described for cold-rolled and annealed samples. Annealing temperatures up to 900°C, which is slightly above the allotropic transformation temperature, were explored. Of interest was the observation that the orientation of the hexagonal-close-packed material after annealing in the temperature range of the stable body-centered-cubic phase was similar to that of the material which had been annealed in the a temperature region, although a change in texture would be expected because of the many new orientations based on an orientation relationship between the two forms of zirconium. The reversion to an original orientation after an allotropic transformation cycle is not unusual. It has been found for titanium,"* for thallium," and for cobaltB among the hexagonal metals. Burgers found in his original work7 that, when zirconium was cooled through the allotropic transformation and then reheated, the body-centered-cubic phase reverted to the original orientation. Additional experimental work has been carried out to further explore the textures of zirconium after annealing in the temperature range above the allotropic transformation. In addition, a reappraisal was made of the earlier results for zirconium&apos; in light of recent work on titanium4 which has shown that the texture type depends quantitatively on the temperature of annealing and that spurious areas may be encountered in the pole figures of hexagonal metals determined by the X-ray spectrogoniometer technique of analysis. Experimental Procedure Crystal-bar zirconium prepared by the iodide process was the material used in this investigation. The major impurity was hafnium which was less than 0.3 pct. The composition obtained by spectro-graphic analysis is given in Table I. Cold-rolled specimens were prepared from crystal bar by a series of reductions of approximately 0.010 in. until the sheet reached a thickness of 0.010 in., after which it was cold rolled to 0.001 in. thickness between sheets of alloy steel. The total cold reduction amounted to about 99.8 pct. Specimens were annealed for % hr at 1000" to 1100" to 1200°C or 1 hr at 1400°C in an evacuated Vycor or quartz tube. The transmission pole figures were obtained by

Jan 1, 1956

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

Jan 1, 1952

By C. B. Alcock, M. G. Hocking

The kinetics of the growth of sulfate layers on blocks of Cu20 has been studied between 688" and 800°C. At 788c the over-all weight increases followed the parabolic rate law, with k = 216 30 sq mg per cm4 min, using a 1:1 entering gas mixture of SO2:02. At 757 after an initial linear period the parabolic rate law was followed, with k = 57.8 10 sq mg per cm4 min. The gas mixture required a platinum catalyst to produce the maximum SOs pressure. The sulfation rate at 757&apos; and 788c was high until all the CUZO had changed into a core of CuO, when it became very much lower. At 757°C marker experiments showed that the sulfates (CuO. CuS04 and CuSO4) grow outwards from the oxide surface, but CuO. CuS04 mixed with CuO was found beneath the markers. At 688 markers were found at the CuO. CuS04/CuS04 interface. Visual observations at 757 showed a liquid eutectic moving beneath the sulfate surface. causing very rapid sulfation and extruding to solidify as thick &apos;needles" up to 8 mm long. Marker experiments have shown conclusi.cely that CuO grows on Cu20 in air by the outward migration of copper. ThermODYNAMIC measurements on the sulfate and basic sulfate of copper, reported recently,&apos; are followed here by measurements of the rates of formation of these sulfates on cuprous oxide, in order to provide a background for the understanding of roasting processes. peretti2 and McCabe and Morgan3 have shown that the phase Cu20 lies next to Cu2S when the sulfide is roasted under conditions where sulfates will be formed. Since this would present too complex a system for kinetic study, the present work4 has been based on the kinetics of sulfation of the oxide phase. The results of a study of the kinetics and mechanism of the sulfation of cobaltous oxide have recently been reported.4,5 Results on the sulfation of cuprous oxide have also appeared,6 but are at variance with those to be reported here. This seems to be because the previous workers6 did not obtain constant SO3 pressures from the SO2/O2 sulfating gas mixtures used, as will be discussed later. Wadsworth, Leiter, Porter, and Lewis found that the sulfates produced when SO2/O2 mixtures are passed over Cu20 at red heats are CuS04 and the basic sulfate CuO.CuSO4. When the decomposition of CuS04 was followed&apos; by differential thermal analysis, a stage corresponding to CuO .CuS04 was reached before decomposition into the oxide occurred. APPARATUS The vertical furnace used for quantitative studies was a conventional resistance-heated and propor- tionately controlled furnace with an even zone (1 deg) which was 4 cm long. The gas mixtures of SO2 and 02 were made by mixing measured flows from capillary flowmeters and drying over phosphorous pentoxide before passing them into the Pyrex top-piece of the furnace assembly. A mullite tube of bore 2% cm was used as reaction vessel and at the bottom of this tube was a trap for SO3, which condensed as a colorless liquid. The residual gas was led into a fume cupboard for ventilation to the atmosphere. The furnace used for visual observations of needle growth and other phenomena consisted of a transparent silica reaction tube of bore 3 cm, having an optically flat silica window sealed into its wall. The reaction tube was clamped vertically, inside a mullite tube of bore 4 cm and length 42 cm which was heated by Kanthal windings. The window in the silica reaction tube was arranged opposite a hole 3 cm wide and 2 cm tall which had been cut in the wall of the mullite winding tube 19 cm from its top end. A binocular microscope was used to look through the window, illumination being provided by a focusing microscope-lamp offset sideways and downwards. The oxide block to be sulfated was suspended from the removable Pyrex top-piece to the reaction tube, by means of which it was inserted at the start of the experiment, and through which entered the S02/02 gas mixture. The variation of the temperature inside the reaction tube with horizontal and vertical displacement from the window was investigated, and, while it can be said that the temperature was constant 1 deg, its value at a given position was known only to 12 deg. In both furnaces, the oxide block to be sulfated was suspended from a small silica hook immediately downstream from a platinum thimble used as catalyst, which was held on a long silica rod from a Pyrex spring attached to the removable Pyrex top-piece of the furnace. The spring was only included in the quantitative sulfating furnace; its sensitivity was 1.4 cm per g and it was found to be free from creep in a 16-hr test when carrying the working load. The extensions were followed by a cathetometer which could be read to 0.001 cm, corresponding to i0.7 mg. Extensions of the spring were measured on adding weights between 5 and 500 mg to the working load (thimble + oxide block), and Hooke&apos;s law was closely obeyed. SAMPLES Cuprous oxide blocks were prepared by oxidizing Johnson Matthey "Specpure" copper sheet of 1 mm thickness (impurities: iron at 3 ppm, silver at 2 ppm, lead, nickel, sodium, and silicon each at 1 ppm, calcium, chromium, magnesium, and manganese each at less than 1 ppm) for 6 days in air at 1000°C in a re-crystallized alumina boat. It has been reported7 that when Cu20 is prepared by heating copper sheet for 1 day the central plane of the blocks produced consists

Jan 1, 1967

By M. Karmis

The development of engineering rock classification systems has received considerable at tent ion during the past few years. The purpose, application and method of assigning an index of rock quality, vary considerably between these systems. Several of them are directed toward the assessment of stability and support potential of an excavation whereas other systems are estimating a particular response of the rock, i.e. blastability or ripability. In the most widely accepted engineering rock classification systems, rock quality is expressed either in terms of meaningful descriptions or by a quantitative evaluation of a geomechanical property or properties. The application of sonic wave parameters in the engineering classification of rock mass and rock material has been the subject of considerable interest amongst investigators. The advantages of utilizing such techniques include minimal sample preparation, capabilities for large scale testing and the ability to perform non- destructive as well as reproducible tests. The purpose of the research presented in this paper was to determine the most appropriate sonic wave parameters for engineering rock classification purposes, to utilize these findings in developing new or modifying existing classification systems and, finally, to apply this information in the prediction and analysis of blasting wave characteristics.

Jan 1, 1984

By M. E. Wadsworth, P. H. Yu, C. K. Hansen

A study of the rate of dissc5lution of chalcopyrite (CuFeS2) in acidic solutions under oxygen overpressures was carried out by measuring the rate of formation of cupric ions in solution. Effects of temperature, oxygen partial pressure, surface area, and concentration of sulfuric acid were evaluated. A sized batch of chalcopyrite was leached in the temperature range of 125° to 175°C and in the pressure range of 75 to 400 psi of oxygen. In 0.5 N H2SO4 all products of reaction went into solution except for trace amounts of elemental sulfur. The dissolution of chalcopyrite followed linear kinetics and was essentially independent of hydrogen ion concentration for H2S04 concentrations between 0.2 and 0.5 N. The oxygen dependence indicated adsorption approaching limiting values with increasing oxygen pressure. The linear mechanism was explained in terms of steady-state adsorption of oxygen at the chalcopyrite surface followed by a surface reaction. The enthalpy of activation for adsorption of oxygen was found to be approximately 33 kcal per mole. An activation enthalpy of approximately 9 kcal per mole was observed for the surface reaction. Charge transfer reactions are not rate controlling in the process.

Jan 1, 1973

By P. Rama Rao, D. H. Sastry, T. R. Anantharaman

Deformation (a) and twin (a&apos;) stacking-fault densities in cold - wor ked filings of fcc silver alloys containing 2, 4, and 6 wt pct Sb have been estimated from Debye-Scherrer peak shifts and asymmetries, respectively. Evidence has been obtained for a possible strain-induced transformation in a two-phase alloy containing 9.0 zut pct Sb. Using Fourier analysis of X-ray line profiles, the effective particle sizes and root mean square strains have been determined for the three fcc alloys in the cold-worked condition. The values of the compound fault probability 0.5a + a&apos;) evaluated from peak shifts and asymmetries are in reasonable apeement with those derived from peak broadening. COLD work of fcc metals may produce both deformation and twin (also called growth) stacking faults, which can be detected and quantitatively estimated by X-ray diffraction techniques.&apos; In addition to peak broadening, deformation faults produce a shift in peak positions and twin faults an asymmetry of the Debye-Scherrer reflections. Besides stacking faults, a reduction in the size of coherently diffracting domains and distortion within these also broaden the powder reflections of deformed fcc metals and alloys. Fourier analysis&apos; of peak shapes provides quantitative infor- mation about the effective domain sizes, lattice strains, and also the compound fault probability (1.5a + a&apos;), where a and a&apos; represent deformation-and growth-fault density, respectively. The Paterson method2 for determination of a from peak shifts, the warren3 or wagner4 method for evaluation of a&apos; from peak asymmetries, and the Fourier analysis for quantitative estimates of all the contributory causes of peak broadening have, in the course of the last decade, been extensively applied to obtain data for a number of deformed fcc metals and alloys. One of the useful results of earlier measurements of a in several solid solutions is a correlation between a and the solute valence as well as electron concentration per atom (p) in alloy systems based on a particular solvent. The work of Smallman and westmacott5 on Cu-Zn, Cu-A1, and Cu-Sn, of Foley, Cahn, and ~aynor&apos; on Cu-Si and Cu-Ge, and of Rama Rao and Anantharaman7 on Cu-Si and Cu-Sb has revealed a common trend in the increase of a with p and also a with valency of the solute. Cahn and Davies&apos; and Ad-ler and wagnerg have observed similar trends for silver alloys containing cadmium, indium, and tin. Data on a for silver alloys with a pentavalent solute element are not, however, available. It is primarily to fill this need that the present investigation on Ag-Sb alloys was undertaken. Utilizing the Patersonand Warren methods, values of a and a&apos;, respectively, have been determined in three silver alloys containing 2, 4, and 6 wt pct Sb. By Fourier analysis of the broadening of Debye-Scherrer peaks, effective particle sizes, lattice strains, and the compound fault probability (1.5a +a&apos;) have also been evaluated.

Jan 1, 1967

By Roy W. Moore

The Tom Reed Extension and Big Jim mines of United Eastern Mining Co. are situated in the Oatman district, Mohave County, Ariz., about 28 miles southwest of Kingman, the nearest railway point. Articles descriptive of the mine surface plant, mill construction, and plant operations have been written by Otto Wartenweiler,&apos; the designing engineer; Wheeler 0. North12 when he was assistant general manager for the company, and Earle M. Bagley, mill superintendent.3 The last article covers average costs for the full time the mill was operated. The geology of the mines is described by F. L. Ransome 4 of the United States Geological Survey. Production was started in January, 1917, and the known orebodies were exhausted in May, 1925, showing a life of seven years and five months. On account of the comparatively short life and the fact that stoping operations were confined to two orebodies, little experimenting was done with mining methods. The two orebodies were in what is generally called the Tom Reed-United Eastern vein, which occupies a fault fissure having a normal displacement of several hundred feet. Seven or eight very productive ore shoots were mined along this vein in a distance of 1 1/2 miles, the two worked by the United Eastern being 1 mile apart. The maximum dimensions of the Tom Reed Extension ore shoot were: height, 750 ft.; length, 950 ft.; thickness, 48 ft. The vein structure varied from a solid quartz-calcite filling to a series of parallel stringers separated by andesite. From this body, 511,976 tons of ore were mined. (Fig. 1.) The maximum dimensions of the Big Jim orebody were: height, 450 ft.; length, 850 ft., thickness, 35 ft. Its structure was similar to that of the Tom Reed Extension but larger sections of the vein were made up

Jan 1, 1928