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By W. L. Austin

At the Steptoe metallurgical plant, where ore of the Nevada Consolidated Copper Co. is beneficiated, a small copper-leaching annex has been in operation treating flue dust from roasting-furnace dust chambers, together with a siliceous oxidized ore. This leaching plant was designed to obviate smelting low-grade siliceous flue dust, which interfered with the operation of the reverberatories by forming a blanket on the charge. The major portion of the copper content of the flue dust accumulating in the upper chambers of the roaster flue, and at the stack, is water soluble, and also contains much free sulphuric acid and soluble sulphates. It was found that sufficient acid could be obtained by mixing this material with water to provide a lixiviant for leaching the siliceous copper ore mentioned. This was the sole source of the lixiviant used in the operation to be described. An analysis of the flue dust showed it to be composed as follows : Per Cent. Copper.............................................. 3.00 siO2................................................. 23.41 Fe................................................... 4.08 CaO + MgO......................................... 2.72 Al203................................................ 0.07 Free H2S04........................................... 19.94 SO3 combined as sulphate.............................. 25.10 H2O combined with the sulphates....................... 10.67 0................................................... 2.50 Total................................... 97.49 Copper soluble in dilute H2SO4.......................... 2.56 The oxidized ore, locally known as carbonate, has the following composition:

Jan 1, 1915

[Holds monthly meetings, except June, July and August, J JOHN A. CHURCH, JR., Chairman JOSEPH E. POGUE, Vice-chairman SIDNEY ROLLE, Vice-chairman EDWARD C, MEAGHER, Secretary, Texas Gulf Sulphur Co,, 41 E, 42nd St., New York M, H, MERRISS, Treasurer, 42 Broadway, New York ARTHUR NOTMAN T. T, READ Boston Meets first Monday of each winter month. EDWARD C. GEITHER, Chairman WILLIAM S. BLACK, Vice- chairman DONALD H, MCLAUGHLIN, Secretary, treasurer, Rotch Bldg,, Harvard Univ,, Cambridge, Mass. J, L. GILLISON A. G, WAITE]

Jan 1, 1928

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York L. W. FRANCIS, Chairman, WILLARD S. MORSE,. Vice-Chairman. THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. P. A. MOSMAN, Treasurer. LOUIS D. HUNTOON. Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. TIMOTHY W. SPRAGUE, HENRY A. WENTWORTH. Columbia F. A. THOMSON, Chairman. GEORGE W. RODDEWIG, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. R. S. McCAFFERY, S. H. RICHARDSON.

Jan 8, 1914

By A. Gemperle

Electron diffraction and transmission electron microscopy on foils at room temperature were used to investigate the ordering of Fe-Si alloys containing 10 to 23 at. pct Si. A certain degree of DO3 order was found in all alloys. With the exception of the lowest silicon concentration for which the antiphase domains could not be clearly resolved, the alloys have a domain structure of two-domain type with boundaries having 1/4a01<111> displacement vectors for less than 12.3 at. pct Si and with boundaries having 1/2 a0<100> displacement vectors for more than 12.3 at. pct Si. The alloys with 12.3 at. pct Si have a domain structure consisting of fine domains with 1/2a&apos;o<100> boundaries within much larger domains with 1/4a&apos;o<111> boundaries. The development of these structures can be explained by transition of the alloy from the disordered state into the B2-type order and then into the D03-type order by the mechanism proposed previously for the FeSAl alloys. The existence of the B2 structure in the lower part of the investigated concentration range reported in some articles can be explained by fine domains with 1/2a&apos;o<100> boundaries formed by several disordered planes within large domains with 1/4a&apos;o<111> boundaries. The ordered structure predicted by the theory —with practically no domain boundaries —is found in the alloys having 12.3 at. pct Si where it develops in the B2 structure region. ORDERING in Fe-Si alloys was first studied by phragmenl who found that beginning with 13 at. pct Si the DO3 (Fe3Si) superlattice reflections appear in the diffraction patterns. The equilibrium diagrams constructed later by corson2 and Haughton3 from various measurements proposed the existence of a homogeneous solid solution (a phase) in the range from 0 to 25 at. pct Si. Jette and Greiner4 and Farquhar et al.5 measured the relation between lattice parameter and composition and they considered the break in the curve at 9 to 10 at. pct Si to be caused by the ordered solution a"(Fe3Si). Glaser and Ivanick6 Determined critical ordering temperatures of the alloys containing from 10.9 to 27.9 at. pct Si from the measurement of the electric resistivity of quenched samples. In all cases the critical temperature was lower than the melting point and it was highest for 25 at. pct Si. Lihl and Ebel7 measured the lattice parameter curves at various temperatures up to 1000°C. The region between two breaks on these curves, corresponding to 10 to 12.5 at. pct Si at room temperature, was considered by them to be two-phase (a + a"). They concluded by extrapolation of the measured values that a" in the alloy having 25 at. pct Si is stable up to the melting point. Davies8 studied superlattice reflections in the X-ray diffraction patterns of an alloy containing 8.7 at. pct Si. He found the B2 structure and short-range order in the slowly cooled samples and the DO3 A. GEMPERLE is Research Scientist, Institute of PhysicS, Czechoslovak Academy of Sciences, Prague, Czechoslovakia. __Manuscript submitted January 2, 1968. IMD structure in the quenched and annealed samples. This investigation first reports the presence of the B2 structure, phase a&apos;: in Fe-Si alloys. Meinhardt and krisement9,10 also found its existence in Fe-Si alloys by neutron diffraction. No order was detected by them in the alloy containing 8 at. pct Si. The onset of B2 order was observed at a composition of 9.2 at. pct Si. They found almost perfect B2-type order with partial DO3-type order at room temperature in the 10 to 12.5 at. pct Si range and almost perfect DO3-type order in the 12.5 to 25 at. pct Si range. They established the critical temperatures Tc of both the structures through measurement at higher temperatures. The critical temperature for the B2 structure was found to be always higher than the critical temperature for the DO3 structure of the same alloy. They extrapolated the curves of the critical temperatures and concluded that the alloys with more than 17 at. pct Si have the B2 structure up to the melting point and the alloys with more than 23 at. pct Si have the DO3 structure up to the melting point. The results of Meinhardt and krisement9,10 were confirmed by Dokken&apos;s measurement" of the temperature dependence of the electrical resistivity in the 10.8 to 15 at. pct Si range. On the other hand chessin12 detected by X-ray diffraction a considerably lower degree of order in the 12.7 at. pct Si alloy. ANTIPHASE DOMAIN STRUCTURE IN ALLOYS WITH B2- AND DO$-TYPE ORDER The ordered structures B2 and DO3 can be described in terms of a subdivision of the bcc lattice into four fcc sublattices with a parameter double that of the bcc lattice. Following Marcinkowski13 we will label them I. 11, 111, IV. The B2 structure in the AB alloy is formed by placing A atoms on sublattices I and II and B atoms on sublattices III and IV. In a non-stoichiometric perfectly ordered alloy having concentration (A) > (B), A atoms occupy sublattices I and 11. and A and B atoms distributed at random occupy sublattices III and IV. The DO3 structure in an A3B alloy is formed by placing A atoms on sublattices I, 11, and 111, and B atoms on sublattice IV. In a nonstoichiometric, perfectly ordered alloy having concentration (A)/3 > (B), A atoms occupy sublattices I, 11, and 111, and A and B atoms distributed at random occupy sublattice IV. As further shown in Ref. 13, two types of domains are possible in the B2 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4 a&apos;o<ll1> only. Four types of domains are possible in the DO3 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4a&apos;o<111> and 1/2a&apos;o<l00>. Bethe14 suggested on the basis of theoretical considerations that in a structure with two sublattices at low temperatures only one domain should be present in the whole crystal at equilibrium. Similarly Bragg15 concluded that at low temperatures the domain struc-

Jan 1, 1969

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York, L. W. FRANCIS, Chairman, WILLARD S. MORSE, Vice-Chairman. THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. P. A. MOSMAN, Treasurer. LOUIS D. HUNTOON. WILLIAM A. POMEROY. Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. ROBERT H. RICHARDS, ALBERT SAUVEUR. Columbia FRANK A. ROSS Chairman. RUSH J: WHITE, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. FREDERIC KEFFER FRANCIS A. THOMSON,

Jan 2, 1915

PROF RICHARD ÅKERMAN Stockholm, Sweden PROF RICHARD BECK Friberg, Germany ANDREW CARNEGIR New York, N.Y. DR. JAMES DOUGLAS New York, N.Y. PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HOFFER Leoben, Austria PROF HENRI LOUIS LE CHATELIER Paris France M FLORIS OSMOND Paris, France ALEXANDRE POURCEL Paris, France JOHN E. STEAD Middlesborugh, England DR. ING H. C. EMIL SCHROEDTER Dusseldorf, Germany JAMES M. SWANK (Associate) Philadelphia, Pa. PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia CHARLES D WALCOT Washingtion D.C.

Jan 1, 1910

Coal Division Mineral Industry Education Division Industrial Minerals Division Minerals Beneficiation Division Mineral Economics Division Mining, Geology and Geophysics Division Council R C Stephenson, Chairman (Ind Min Div), M D Cooper (Coal), H F Yancey (Coal), S D Michaelson (MBD), Will Mitchell, Jr (MBD), J R Van Pelt, Jr (MIED), S S Cole (Ind Min Div), J D Forrester (MGGD), L E Shaffer (MIED), E L Clark (MGGD), C W Merrill (MED), E H Robie, Acting Secretary, 29 West 39 Street, New York 18, New York

Jan 1, 1955

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York L. W, FRANCIS, Chairman, WILLARD S. MORSE, Vice-Chairman. THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. P. A. MOSMAN, Treasurer. LOUIS D. HUNTOON. Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. TIMOTHY W. SPRAGUE, HENRY A. WENTWORTH. Columbia F. A. THOMSON, Chairman. GEORGE W..RODDEWIG, Vice-Chairman. LYNDON K, ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. R. S. McCAFFERY, S. H. RICHARDSON.

Jan 7, 1914

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York L. W. FRANCIS, Chairman. WILLARD S. MORSE, Vice-Chairman. . THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. P. A. MOSMAN, Treasurer. LOUIS D. HUNTOON, Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. TIMOTHY W. SPRAGUE, HENRY A. WENTWORTH. Columbia F. A. THOMSON, Chairman. GEORGE W. RODDEWIG, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. R. S. McCAFFERY, S. H. RICHARDSON.

Jan 6, 1914

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York L. W. FRANCIS, Chairman, WILLARD S. MORSE, Vice-Chairman. THOMAS T. READ, Secretary, Woolworth Bldg., New York. N. Y. P. A. MOSMAN, Treasurer. LOUIS D. HUNTOON. Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. TIMOTHY W. SPRAGUE, HENRY A. WENTWORTH. Columbia F. A. THOMSON, Chairman. GEORGE W. RODDEWIG, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. 0. Drawer 2154, Spokane, Wash. R. S. McCAFFERY, S. H. RICHARDSON.

Jan 9, 1914

EXECUTIVE COMMITTEES OF LOCAL SECTIONS New York L. W. FRANCIS, Chairman. WILLARD S. MORSE, Vice-Chairman. THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. P. A. MOSMAN; Treasurer. LOUIS D. HUNTOON. WILLIAM A. POMEROY Boston HENRY L. SMYTH, Chairman. ALFRED C. LANE, Vice-Chairman. AUGUSTUS H. EUSTIS, Secretary-Treasurer, 131 State St., Boston, Mass. ROBERT H. RICHARDS, ALBERT SAUVEUR. Columbia FRANK A. ROSS, Chairman. RUSH J. WHITE, Vice-Chairman. LYNDON K. ARMSTRONG, Secretary-Treasurer, P. O. Drawer 2154, Spokane, Wash. FREDERIC KEFFER, FRANCIS A. THOMSON.

Jan 1, 1915

First actual production of titanium metal at the newly constructed Henderson, Nev., plant of Titanium Metals Corp. of America occurred in mid-October. Production will be expanded rapidly until the initial goal of 10-tons per day is reached. This will be equivalent to eight times the present world production of titanium metal. W. Eberstady & Co., New York City, has announced plans for construction of a $400 million plant for the manufacture of synthetic liquid fuels from coal in southern Illinois, if the Government will guarantee a minimum price for the gasoline and other products to be produced.

Jan 11, 1951

By AIME AIME

In taking account of stock, on the occasion of the recent removal of the office of the Institute, it was found that pamphlet copies of the papers named in the list given below were on hand, in excess of the average number deemed adequate for future casual demand. Special reduced rates will be made for these surplus copies to members applying promptly. "First come; first Served." Author. Title. Ref. No. ASHBURNER, C. A. " Petroleum and Natural Gas in New York State." 273 MARTENS, A. "The Microstructure of Ingot¬ Iron and Cast Ingots." 626

Jan 1, 1907

By A. H. Larson, R. J. McClincy

The activity of Sb,03 in PbO-Sb,03 slags containing less than 50 mol pct Sb,03 was determined by the inert-gas saturation method at 700°C. In this composition range, the activity gf SbzO3 shows a strong negative deviation from ideality. The activity of PbO in these slags was calculated by application of the Gibbs-Duhem iniegration to the Sb203 activity data. The calculated activity of PbO in slags containing more than 63 mol pct PbO was found to deviate in a positive direction from ideality uthile a negative deviation was found for slags containing less PbO. The standard Gibbs free energies of formation of Sb,03 and PbO. Sb203 have been calculated and compared with existing data in the literature. The activity of Sb203 in PbO-Si0,-Sb203 (PbO/SiO, = 2) slags containing less than 25 mol pct Sb,03 was also determined by the inert-gas saturation method at 700°C. In this composition range, the activity of Sbz03 shows a very large negative deviation from ideality. VERY little experimental work has been published in the past to determine equilibrium data in the oxide systems connected with the refining of lead. These data are of value since impurities such as antimony, arsenic, and tin must be removed from lead and recovered for further treatment. Equilibrium studies on antimony and arsenic systems are also of interest for the design of new processes for lead refining and lead dross treatment. Maier and ~incke&apos; first determined the liquidus curves for the PbO-Sb203 system and identified the compound PbO . Sb203. They found the phase diagram for this system to be two simple eutectics located on either side of the congruent melting compound. They also determined a very limited amount of vapor pressure data for Sb406 abbve PbO-Sba3 melts at 697"~. A second phase diagram investigation on this system was reported by Hennig and Kohlmeyer&apos; who confirmed the existence of the compound PbO . Sb203 as well as the form of the diagram. A disagreement was noticed, however, in that their liquidus temperatures over nearly the entire composition range were higher than those reported by Maier and Hincke. Barthel~ and pelze14 redetermined the liquidus curve at the PbO-rich end of the PbO-Sb@, system and agreed very closely with the results of Maier and Hincke. None of the investigators mentioned above reported any mutual solid solubility in the PbO-SbD3 system. Zunkel and Larson5 have determined the phase diagram for the PbO-rich end of the PbO-Sb203 system by slag-metal equilibrium studies in the Pb-PbO-Sb203 system and by thermal analysis studies in the PbO-Sbz03 system. A maximum solid solubility of 5.6 mol pct Sb203 in PbO was observed at the eutectic temperature of 604°C. Their results for the phase diagram agree favorably with those of Maier and Hincke. The vapor pressure of Sb2O3 in the temperature range from 470" to 800°C has been determined by Hincke, using a modification of the transportation meth~d.~ His results for temperatures below the melting point of Sba3 are the only data reported in the published literature. The predominant vapor species has been shown to be Sb,06 by Norman and staley.? Myzenkov and Klushin,8 using the boiling-point method, have determined the pressure of Sb406 above liquid SbD3 in the temperature range from 715" to 1025°C. The agreement between these two studies is not very close. A portion of the discrepancy lies in the fact that Hincke used silica crucibles, which were attacked by the liquid Sbz03 at high temperatures. This fact does not account, however. for the large difference observed at the melting point. ~aier&apos; gives a brief summary of vapor pressure data for Sb,O, above pure liquid Sbz03 which agree quite well with the data of Myzenkov and Klushin at temperatures near the melting point. This paper describes the determination of Sb2O3 activity data in the PbO-Sb203 and Pb0-Si02-Sb203 (PbO/SiOz = 2) systems by the inert-gas saturation method. These activity data are compared with the data calculated by Zunkel and arson. EXPERIMENTAL Materials. The materials used in this investigation were analytical reagent-grade PbO (99.8 pct PbO, 0.14 pct insoluble in CHsCOOH, 0.02 pct not precipitated by HB, 0.1 pct CaO, and 0.08 pct SiOz), Sbf13 (99.6 pct Sb203, 0.004 PC~ C1-, 0.005 PC~ SO;-, 0.15 p~t AS, 0.001 pct Fe, and 0.03 pct other heavy metals such as Pb), and SiOz (chromatographic grade). Apparatus for Vapor Pressure Determinations. The apparatus used in this investigation consisted of a transportation reaction system with two separate gas trains. The argon transporting gas was first mixed with a small amount of hydrogen, metered, and dried by passage through silica gel and anhydrone drying tubes arranged in series. After this preliminary drying, the argon was passed through copper wool at 500°C to convert the residual oxygen to water vapor which was removed by three anhydrone drying tubes. A second stream of argon was metered and dried and then passed around the outside of the alumina reaction tube to flush away the volatile species to pre-

Jan 1, 1970

The second special war meeting of the New York Section was held on Thursday evening, Aug. 23,-preceded by is an informal dime The topic for discussion -was the supply of sulphur and pyrite, the raw materials for the manufacture of one of the most important of till war materials-sulphuric acid. The first speaker was William Young Westervelt, the Institute&apos;s representative on the War Minerals Committee. Before taking up the subject of the evening, Mr. Westervelt briefly described the organization and plan of operation of the War Minerals Committee.

Jan 10, 1917

By John T. Ryan

DEFINITE improvement in its accident fatality rate in the coal-mining industry was recorded during 1941, based on preliminary figures for the period from January through October. Total production during this ten-month period was approximately 91 percent of the total production in all of 1940. The ten-month accident rate for both bituminous and anthracite mining in 1941 was 2.15 killed per million tons of coal mined, compared with a rate of 2.66 for the full year of 1940. The bituminous rate decreased from 2.55 in 1940 to 1.99 in ten months of 1941, and the anthracite rate from 3.62 to 3.53 in similar periods. The decrease is more apparent for the bituminous branch of the industry, as the high figure in 1940 was due to seven major disasters which brought death to 276 men. The same number of major explosions during ten months of 1941 caused only 64 lives to be lost. The severity of the explosions has been lower this year but a definite need still exists for reduction in this type of accident.

Jan 1, 1942

We the undersigned, being all persons of full age and citizens of the United States and a majority residents of the State of New York, desiring to form a corporation pursuant to the provisions of the Membership Corporations Law for the purpose of incorporating, as provided in Section 5 of Article I. of said law, the existing unincorporated association known as American Institute of Mining and Metallurgical Engineers, Incorporated, do hereby make, acknowledge and file this Certificate for that purpose, and do Certify as follows: I. That the American Institute of Mining Engineers is an unincorporated association organized and existing with the object of promoting the arts and sciences, connected with the economic production of the useful minerals and metals and the welfare of those employed in these industries by means of meetings for social intercourse and the reading and discussion of professional papers, and to circulate by means of publications among its members and associates the information thus obtained. II. That the persons duly appointed or designated to manage the affairs of said association are designated by the rules thereof Members of its Council; that the undersigned are all members of said Council as the same was constituted on the 29th day of December, 1904. III. That on said last-mentioned date a regularly called meeting of said association was held at its office in the Borough of Manhattan, City of New York; that thirty days before such meeting notice of the intention to incorporate said association was given by mail to each member thereof whose residence or post-office address is known; that at said meeting the following resolutions were offered, seconded and duly adopted by the unanimous vote of all its members then present, to wit: "Resolved, That it is the sense of the members and associates of the American Institute of Mining Engineers in general meeting assembled that it is desirable and necessary for the well being of said association and its members and for the furtherance of the objects for which the same has been formed, that said association incorporate under the Membership Corporations Law of the State of New York; "And Further Resolved, That the Members of the Council of this Association, or a majority thereof, be and they hereby are authorized, in accordance with the provisions of Section 5 of Article I. of the Membership Corporations Law, to incorporate this association for the same purposes for which it has been organized and conducted, in the manner provided in Article II. of said law;, "And Further Resolved, That the name of said corporation as hereby adopted by this meeting shall be American Institute of Mining Engineers; "And Further Resolved, That the said incorporators shall be named in the Certifi¬cate of Incorporation as directors of such corporation until its first annual meeting,

Jan 1, 1940

PROF RICHARD ÅKERMAN Stockholm, Sweden DR FRANK DAWSON ADAMS Montreal, Canada ANDREW CARNEGIR New York, N.Y. PROF HATON DE LA GOUPILLIERE Paris, France SIR ROBERT A. HADFEILD London, England HERBERT C. HOOVER Leoben, Austria JAMES FURMAN KEMP New York, N.Y. PROF HENRI LOUIS LE CHATELIER Paris France EZEQUIEL ORDONEZ Mexico City, Mexico ALEXANDRE, POURCEL Paris, France PROF RICHARD H, RICHARDS Boston Mass. JOHN E. STEAD Middlesborugh, England PROF DIMITRY CONSTANTIN TSCHERNOFF St Petersburg, Russia PROF TSUNASHIRO WADA Tokyo, Japan CHARLES D WALCOT Washingtion D.C.

Jan 1, 1923

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&apos; 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 A. Singh, W. M. Fleming, J. J. Santana, A. E. Torma

The present study investigated the extraction of uranium from a low-grade ore by sulfuric acid and the removal of radium from the leach residues by brine solutions. The optimum leaching conditions were found to be 1.5 mole [£]-1 H2SO4, 6.Og[9]-1NaClO3, 75°C,50% pulp density and 750 rpm with respect to the rate of uranium extraction. The maximum theoretical attainable rate of uranium extraction was determined to be V = 1.09 x 10 -2 mole [¢]-1h-1 with respect to pulp density. The order of reaction was found to be zero regarding the effect of sodium chlorate concentrations. The apparent activation energy of uranium extraction was calculated from the Arrhenius plot to be [A]E a - 2.36 kcal mole-1 (9.87 kJ mole-1). Based on a statistical design, an empirical equation has been developed describing the rate of uranium extraction with the leaching parameters. This equation can be used to generate data which may be useful for scaling up the process to pilot plant level. The most efficient brine solution for the extraction of radium - 226 from the leach residue was found to contain one mole[f] -1 CaCl2 and 0.01 mole [2] -1 HC1. The two step leaching with this solution resulted 87% removal of radium from the leach residue. On the basis of this study, a flow-sheet has been proposed for the extraction of uranium and radionuclides from the ore and leach residue to yield almost innocuous tailings.

Jan 1, 1982