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By Yi-Shen Li

This report has been prepared by Lockheed Missiles & Space Company, Inc. (LMSC), under United States Bureau of Mines Contract No. H0220040 dated 21 June 1972 for the design, development, fabrication, and certification of the One-Hour Self-Rescue Breathing Apparatus (PBA). The PBA is a self-contained, oxygen-generating, CO2-removing closed-loop breathing apparatus that provides a minimum of 1 hour of breathable atmosphere during escape from a mine with a contaminated or oxygen-deficient atmosphere. This Cost-Plus-Fixed-Fee (CPFF) contract has been successfully completed in a three-phase program. The Phase I tasks included the design, development, and fabrication of prototype units developed at LMSC in accordance with the requirement of the Code of Federal Regulations (CFR) Title 30, Chapter 1, Subchapter B, Part 11 (Appendix A), and was submitted to the National Institute for Occupational Safety and Health (NIOSH) for joint NIOSH and Bureau of Mines certification testing.

Jan 1, 1974

By P. E. Busby, C. Wells, M. E. Warga

Fundamental data on the rate of diffusion of boron in austenite and solubility of boron in the a and y phases of iron and steel have been obtained from deboronizing experiments and provide partial explanations for some of the phenomena observed in boron steels. The rate of diffusion of boron is about the same as carbon in austenite. The solubility of boron in austenite at normal heat-treating temperatures is less than 0.001 pct. A partial tentative Fe-B phase diagram in the important low boron concentration ranges and an equation representing the diffusion of boron in austenite are presented. A LTHOUGH a search of the literature revealed ALTHOUGHthat boron diffusion had not been studied quantitatively and systematically prior to 1948, a few qualitative observations which were made by following the diffusion of boron into iron packed in ferro-boron1-3 suggest that boron obeys normal diffusion laws and that the rate of diffusion increases with increasing temperature. The claim of Cornelius and Bollenrath1 that boron does not appear to influence the rate of carbon diffusion has recently been substantiated by Wells, Batz, and Mehl.4 Calculations based on data from the paper by Campbell and Fayv indicated that the diffusion coefficient (D) for boron in iron at 900°C is approximately 3x10 sq cm per sec; a value of 2x10-7 sq cm per sec at 1038°C has been reported by Digges et al in connection with decarburizing experiments on a commercial boron steel containing 0.43 pct C. During the period 1948 to 1950 several diffusivity constant (D) values for the diffusion of boron in the y phase of iron and steel and a number of solubility values for boron in both a and y phases were reported. It was concluded tentatively as a result of Metals Research Laboratory studies that D values for boron in y and a phases are about the same as for carbon in the comparable phasesa and that carbon up to 0.4 pct did not affect the rate of diffusion of boron in y iron above 1000°C within the limits of experimental error. Whether saturation of the y or a phases with carbon would significantly affect rates of diffusion of boron through them was then and still remains in doubt. The best estimate of Q (activation energy) was reported to be about 25,000 cal, somewhat lower than that for carbon in y iron. The solubility of boron in y iron at 1000°C was thought to be higher than 0.004 pct B but not as high as a more recent analysis of available data shows it to be. The solubility of boron in a iron at 700°C was reported to be 0.0004 pct B, but it would not have surprised the authors if the true solubility value is actually lower than this. Breaks in diffusion curves which were not understood when first obtained prior to 1950 have now been recognized as indicating solubility limits, and these are included in the present paper. Experimental Procedure Two methods were employed in an effort to determine diffusion coefficients (D) for boron in austenite. Early experiments involved the use of welded couples prepared in accordance with the procedure of Wells and Mehl,' but when the results of these experiments proved to be unsatisfactory for calculating D values, studies were continued by means of deboronizing experiments. In both cases, boron analyses following the diffusion anneal were carried out spectrographically and all D values were computed using the Grube solution of Fick's law. The precision of the spectrographic method used proved to be about equal to that reported by Corliss and Scribner" —average deviation from the mean about 5 pct of the amount present when the boron content is 0.003 pct. Concentration-penetration curves obtained from spectrographic analyses of welded couples generally indicated that practically no boron was transported across the weld interface during the diffusion anneal. Furthermore the concentration-penetration

Jan 1, 1954

By Xiao-hui Fan, Xu-ling Chen, Xiao-xian Huang, Gui-ming Yang

Grate-kiln-cooler is a predominant process of producing iron ore pellets in China. Since this process is of multi-variant, strong coupling and large hysteresis characteristics, a reliable performance monitoring is thus essential to ensure product quality and economic benefits. Aiming to efficiently monitor the pellet induration within this process, this study proposed an approach that combines statistical analysis and quality soft-measurement. Soft-measurement of pellet quality was accomplished based on the predicted time-temperature profile, and the soft-measured indices were on-line monitored using statistical control charts. Based on the proposed approach, a monitoring system for grate-kiln-cooler thermal process was developed for a domestic pelletizing plant. Running results demonstrate that our system can assist in the detection or diagnosis of abnormal thermal state and finally helps to stabilize the pellet production.

Jan 1, 2016

By W. Dietzel

Fracture mechanics based techniques are used to gain insight into the phenomenon of stress corrosion cracking (SCC) and to develop guidance for avoiding or controlling SCC. From constant extension rate experiments under rising load or rising displacement conditions the susceptibility of high strength steels, aluminum, magnesium and titanium alloys to SCC and hydrogen embrittlement can be assessed. Such tests on pre-cracked specimens are also well suited for studying the mechanisms leading to SCC by employing appropriate models for the degradation of metallic materials which take into account the uptake of atomic hydrogen from the corrosive environment. Measurements of crack growth resistance curves using the crack tip opening displacement as fracture parameter can be compared with simulated R-curves obtained from modeling of the mechanism of hydrogen embrittlement. The materials investigated are a high strength steel and a magnesium alloy both exposed to environmental conditions which fostered the uptake of hydrogen.

Jan 1, 2010

By John C. Cook

This was a study to identify and evaluate known technologies employing electromagnetic resonance phenomena in solid minerals for their identification and assaying, particularly assay logging of exploratory boreholes. A comprehensive literature search and study revealed some little known NMR (nuclear magnetic resonance) techniques developed by Professor G. J. Béné's group at the University of Geneva, Switzerland. These are suitable for use in weak, inhomogeneous magnetic fields. Laboratory NMR tests of numerous U.S. ore minerals showed good identifying signals from phosphates, fluorspar, bauxite, oil shale, and spodumene (lithium) ores, but not from the copper, lead, antimony or manganese ores tested. Use of EPR "signatures" for such ores is suggested. A conceptual design for an NMR assay logging system is proposed.

Jan 1, 1978

By Richard E. Thill

Two Cross-borehole systems were developed by the Bureau of Mines, one operating at a central frequency of 20 kHz for close-in spacing between boreholes (2-20m) and another operating at a dominant frequency between 1-2 kHz for more distant range (40-300+m) between boreholes. The systems are specially designed for the expected ranges and high resolution required in mining applications. Potential applications of the crosshole systems are presented for a variety of geophysical measurements related to underground mining problems.

Jan 1, 1989

By I. Gaballah

Cadmium is toxic to plant, animals and humans. The council directive of the European Communities No 8315 13lEEC has fixed an upper limit of 200 ppb for the release of cadmium in industrial effluents. The conventional method of neutralization/prccipitation ( NIP ) is inefficient to reach this limit. The objective of this study is to test the efficiency of the trees modified bark to remove cadmium cations from industrial effluents after the conventional treatment by NIP. Laboratory scale tests with synthetic solutions show that the cadmium removal depends upon pH and initial concentration. About 99.9 %, 99 % and 96 % of the metal are removed from synthetic solutions containing 10, 100 and 1000 ppm respectively. Pilot plant trials ( 1 m3 ) with an industrial effluent bearing about 500 ppb of cadmium lead to the almost complete elimination of the cadmium ( final concentration is lower than the analytical detection limits < 20 ppb ).

Jan 1, 1994

By S. V. Volkova, S. V. Mamonov, T. P. Dresvyakyna

"The purpose of the work is complex processing of sulphide-magnetite ores with the separation of iron into iron concentrate, copper and noble metals into copper concentrate.The work shows the research results of the material composition of the sulfide-magnetite ore in the South part of the Peschanskoye deposit. According to the research results it is found that ore contains 0.59% of copper, 66% of which is related to chalcopyrite; 39.9% of iron, 81% of which is magnetite and 3.87% is sulfur, 42% of which is associated with pyrrhotite, 65% of which is a monoclinic modification. According to the results of the mineralogical analysis, it is found that the main iron-containing mineral in the ore under study is magnetite, the content of which is 45%. In addition to magnetite, iron is found in carbonates, pyroxenes, amphiboles, chalcopyrite, pyrrhotite and pyrite. The main copper mineral in the sample is chalcopyrite; covellite, chalcosine, bornite have a subordinate value. The total content of copper minerals in the sample is about 1%. The processing technology provides the three-stage grinding of the ore to a size of 65% of the class-71 µm; a cycle of copper flotation; a cycle of pyrrhotite flotation; wet magnetic separation of flotation hosts. The following optimal parameters are established for the ore under study: the alkalinity of the slurry is 250-280 g/m3 of free calcium oxide in the liquid phase of the slurry; the duration of the main copper flotation is 20 min; the consumption of butyl potassium xanthate is 20 g/t; the consumption of the foam generator T-92 is 15 g/t; the consumption of copper sulfate for the activation of pyrrhotite is 300 g/t; the magnetic field strength is 1500 Oersteds.A complex flotation-magnetic technology for the enrichment of sulfide-magnetite ore has been developed in the laboratory in order to produce a copper concentrate containing 21.6% of copper with 91.7% extraction and an iron concentrate with 66.5% of iron mass fraction and 1.2% of sulfur with an extraction of iron into the concentrate of 87.9%."

Jan 1, 2018

By R. R. Sayers

TWO serious hazards from coal dust confront the bituminous-coal miner- -a physical or safety hazard and a physiological or health hazard. The first threatens the miner with loss of life from coal-dint explosions, and the second with loss of health and earning capacity from inhaling large quantities of the dust. Studies by the Bureau of Mines have shown that coal dust, except some grades of anthracite dust, is capable of initiating an explosion when no explosive gas is present and that its property of extending or propagating an explosion has been responsible for nearly all the widespread explosions that have occurred in bituminous mines in the United States in the present century. For years many mining people believed that low-volatile coal dust was not explosive but not only is it explosive but if the source of ignition is intense, it is as explosive as the dust of many high-volatile coals because the war is creating increased pressure for greater coal production and because of the trend toward greater mechanization in mines, explosion and health hazards from coal dust are likely !n increase considerably.

Jan 1, 1943

By P. D. Merica

The remarkable phenomena exhibited by the aluminum alloy known as duralumin were discovered during the years 1903-1911 by A. Wilm1,2 and have been described by him and by others. 3 4 5 6 The unusual feature of this alloy is the fact, as was shown by Wilm, that it can be hardened quite appreciably by quenching from temperatures below its melting point followed by aging at ordinary temperatures, which consists merely f allowing the material to stand at these temperatures. The hardness is not produced by the quenching alone but increases during the period of aging, which may be from one to three days. Cohn3, 5 gives data showing the increase of hardness of duralumin during aging, after quenching in water from about 450° C. Upon annealing, the alloy so hardened by aging is softened exactly as is hardened steel. The composition of this alloy usually varies within the following limits: Copper, 3 to 4.5 per cent.; magnesium, 0.4 to 1.0 per cent.; manganese, 0 to 0.7 per cent.; aluminum, balance; iron (as impurities), 0.4 to 1 per cent.; silicon, 0.3 to 0.6 per cent. Its density is about 2.85. It is used only in the forged or rolled condition. This alloy has been produced for some years commercially and is in demand for the fabrication of parts for which both lightness and strength are required, such as for aircraft. Its tensile strength will average 50,000 to 60,000 lb. per. sq. in. (3515 to 4218, kg. per sq. cm.) after appropriate heat treatment, such as that described by Wilm.

Jan 6, 1919

By Etienne S. Bieler

Mr. Chairman, Ladies and Gentlemen, I come to you tonight distinctly as a physicist, not as a geologist or a mining man. My experience in applied geophysics has been short, and I do not doubt that many of you have a much larger acquaintance: with the subject than I have. A little over a year ago, the firm of Alderson, MacKay & Armstrong decided to investigate the possibility of developing a new method of electrical prospecting suitable to our northern Quebec and northern Ontario conditions, and asked me to take up the work. A preliminary survey of existing literature convinced me that the field of induction methods was most promising. I wish to give you some account of the work carried on last summer in the Rouyn district in this connection with the very able assistance of Mr. H. G. I. Watson. Geophysical methods of prospecting can be divided generally into four classes: magnetic, electrical, gravitational, and seismic. Each class depends on the existence of a definite property in which the valuable mineral to be discovered differs materially from the surrounding rocks. In the four classes, the property will be, respectively, magnetic permeability, electrical conductivity, density, and elasticity. By far the largest differences occur in the case of electrical conductivity, where it is not rare to find ratios of the order of several millions, or even billions, between ores, sulphide ores especially, and the surrounding rock. Hence the sensitiveness and delicacy of electrical methods. Of these four classes, only two, the electrical and the magnetic methods, have been put to extensive practical use in the discovery of metallic ores. The other two classes are important mainly in connection with oil detection.

Jan 1, 1928

By E. A. Schmidt

The Thompson Creek molybdenum deposit is located in the Bayhorse mining district about 20 air miles southwest from Challis, Idaho. Cyprus Mines Corporation began exploration on the property in 1968, and at present is in the pre-production stripping phase. Molybdenum mineralization is contained in a late Cretaceous (88 m.y.), composite, biotite granodiorite-quartz monzonite intrusive complex. The complex intruded carbonaceous argillites, causing local silicification and hornfelsing of the sedimentary rocks. The main portion of the orebody is unconformably overlain by up to 1000 ft of Challis volcanic rocks (49 m.y.). Surface mineralization and related rock alteration can be recognized over a 2500- x 8000-ft area extending northwesterly from the discovery outcrop. Molybdenite occurs in a network of subparallel quartz-biotite-muscovite-orthoclase veins and veinlets within the intrusive rocks. The zone of +0.020/0 Mo mineralization outlines a steeply dipping tabular configuration in the main orebody and gradually changes into a hood-shaped configuration along strike to the northwest. The overall grade [ ] of the deposit is controlled by the abundance of the quartz- molybdenite veins and veinlets in the intrusive rock. Very little disseminated mineralization is present, and no economic mineralization occurs in the argillaceous sedimentary rocks. Muscovite, biotite, and orthoclase/microcline define three alteration zones that conform with the overall zone of mineralization. The upper alteration zone contains dominantly muscovite and sericite associated with quartz veins. The central zone contains coarse biotite and locally orthoclase and microcline. Molybdenite is most abundant within this zone. The lower zone contains thin envelopes of orthoclase/microcline around quartz veins. Based on about 313,000 ft of drilling and 8592 ft of underground development work, computer-derived ore reserve calculations indicate 200 million tons averaging 0.1 1% Mo at a 0.050/0 Mo cutoff grade with a waste to ore stripping ratio of about 3:l.

Jan 1, 2013

British Coal has made a practical progressive approach to improving the reliability of its mining equipment. Reliability must be addressed at the specification stage but does not end there and routine procedures are used to procure equipment of adequate reliability. The techniques used to monitor and improve reliability during the operational phase of the equipment, providing engineers and operators with detailed printouts, together with the types of maintenance employed, ensure high levels of availability. Finally, the methods of repair and overhaul of British Coal equipment and systems ensure that the initial reliability targets outlined on the specification, can still be achieved.

Jan 1, 1991

By Hugh M. Wolfin

This Information Circular is an abstract of a manuscript which was completed in June 1933, by Mr. Hugh M. Wolflin, formerly of the U. S. Bur eau of Mines. This abstract has been prepared by Charles Will Wright for presentation at the February meeting of the American Institute of Mining and Metallurgical Engineers in New York. It has been necessary to omit many of the details and most of the cost data and tables, as well as the illustrations in the original manuscript. As the use of airplanes in mining developments is making such progress and as a publication on this subject to be of greatest value should include the most recent information, it is unfortunate that, due to a lack of printing funds, it has not been possible to publish this manuscript. The purposes of Mr. Wolflin&apos;s paper are: (1) To describe briefly what has been accomplished in some outstanding examples by the use of aircraft in the mining and petroleum industries, (2) To record costs, (3) To present available information and suggestions to assist in solving future air-transportation problems in the industries under consideration.

Jan 1, 1934

The Bureau of Mines, U.S. Department of the Interior, devised a flotation technique for upgrading chromite in chromium ores and gravity concentrates. The technique consisted of cationic flotation of chromite from a slime-free pulp acidified to pH 2.5 or lower using H2S04 modifier. Flotation results showed that ore containing serpentine as the primary gangue mineral was more amenable to concentration by this technique than ore containing the readily floatable olivine as the primary gangue mineral. Rougher flotation of a chromite ore containing abundant serpertine increased the grade form 19 to 41 percent Cra03 at a chromite recovery of 89.6 percent. Rougher flotation of ore containing abundant olivine upgraded the chromite from 23.4 to 29.6 percent Cr203 at a recovery of 89.4 percent. The technique was also applied to chromite gravity concentrates to further upgrade chromite and to reject silicates. Flotation of a gravity concentrate containing 40.9 percent Cr203 and 4.4 percent SiO2 recovered 90 percent of the chromite in cleaner products containing 44.9 percent Cr203 and 0.63 percent Si02. The combined recovery by gravity and flotation was 87 percent. An economic evaluation of this technique will be undertaken to deter-mine its feasibility for commercial use.

Jan 1, 1980

SOUTHERN CALIFORNIA SECTION Executive Committee SEELEY W. MUDD, Chairman. C. COLCOCK JONES, Vice-Chairman. FREDERICK J. H. MERRILL, Secretary-Treasurer, 631 Higgins. Bldg., Los Angeles, Cal. RALPH ARNOLD A. B. CARPENTER A. B. W. HODGES WILLIAM F. STAUNTON The third meeting of this winter season tool: place in a private dining room of the Sierra Madre Club in Los Angeles on Feb. 1, 1916, at 6:30 p.m., 22 members and guests being present. In the absence of the Chairman, S. W. Mudd, the Vice-Chairman, C. Colcock Jones, presided. After an enjoyable dinner the meeting was called to order, and the first paper by Ralph Arnold on Conservation of Oil and Gas in the Americas was read by the Secretary. W. F. Staunton then read an important paper on The Influence of California Oil on the Mining Industry of the West. In this he touched upon the uses of oil as a fuel for generating power, especially in connection with the Diesel engine. This paper was discussed it some length by J. F. Mitchell-Roberts, R. B. Moran, F. H. Asbury and L. D. Godshall. The Chair then introduced Robert B. Moran of the California State Mining Bureau, Deputy Supervisor of Gas and Oil, for the&apos; Los Angeles . District, who addressed the meeting on the work of his department. The meeting concluded with A. B. Carpenter&apos;s reading of a paper on The California Gasoline Industry by W. R.. Hamilton, Manager of the Ventura Refining Co. F. J. H. MERRILL, Secretary. ,

Jan 4, 1916

By C. H. Riggs

This report describes the geology and reviews the oil-production history of the Dutcher sands of Pennsylvania age in the Muskogee oilfield. The geology and production history are presented not alone as a review of the past behavior of the field but also to interpret the possibilities for future production of oil from semidepleted sands in this and similar areas. The Muskogee field, one of the oldest oil-producing areas in Oklahoma, yields paraffin-base oil of 40° API gravity -a gravity higher than that of most Oklahoma oils. Oil was discovered in the townsite of Muskogee in 1894 but was not produced in commercial quantities until 1904. A peak yearly rate of 1,340,000 barrels of oil was attained in 1910 (see table 1).

Jan 1, 1959

SUGGESTIONS that existing schools give instruction bearing on the mineral industry, or that schools for that purpose should be established in the United States, began to be made early, and it would require too much space to catalogue them all. Some of the more important may be mentioned to indicate their general character. In the "advertisement to such parents as have now (or expect to have) children prepared to be educated in the College of New York," which appeared in the New York Mercury of June 3, 1754, Samuel Johnson, the first president of King&apos;s College, the predecessor of Columbia, said that it was the "design of this college to instruct and perfect the youth," among other things, "in the arts of Numbering and Measuring of Surveying, and Navigation and Geography. . . . and in the Air, Water and Earth around us, and the various kinds of Meteors, Stones, Mines and Minerals, Plants and Animals; and in the knowledge of all Nature in the Heavens above us, and of everything useful for the Comfort, Convenience and the Elegance of Life . . . " Though the concept that natural science should be used to enlarge the bounds of human life was thus implicit at Columbia from the , very beginning (John Stevens graduated from it in 1768, James Renwick in 1807, Horatio Allen in 1833, and A. W. Craven in 1899), it was only during the period of Renwick&apos;s professorship of Natural and Experimental Philosophy and Chemistry (1830- 1853) that much attention was given to applied science.* Among the Austin papers, published by the American Historical Association,~ there is a draft in Stephen F. Austin&apos;s handwriting of a proposed memorial from the legislature of , Missouri to Congress, not only urging "the propriety and utility * See chapter 4 for early interest in this subject in Philadelphia.

Jan 1, 1941

Mineral Sands - "An Industry for the Future"The mineral sands industry is matched only by the gold industry in relation to its current buoyancy. The strong demand for the various mineral sands products, creates a positive environment in which to review the technical and commercial factors affecting the future of this industry. This conference is clearly being held in the right place at the right time.My role today is to put forward a few ideas that may help Australia to assert its rightful role as a major downstream player in an industry which it has dominated for 25 years as a raw material supplier.

Jan 1, 1986

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