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By A. A. el-Geassy, A. A. el-Tawil, Hesham M. Ahmed, Bo Bjorkman

The Iron and steel industry is one of the most intensive energy consuming processes. The majority of iron making processes is now directed towards the uses of fossil-based energy sources like coke, coal and oil. Recently, emphasis has been paid to replace part of fossil- based energy sources with renewable biomass-derived reducing agents. In the present work, the possibility of the effective use of woody biomass in carbon-iron oxide composites was investigated. Wood powder was carbonized in N2 atmosphere at 300 up to 450oC. The carbon content in the produced bio-char increased with temperature. The porosity of the char arises from maintaining the cellular structure inherent in wood biomass increases with temperature. The reduction behavior of four iron oxide-bio char composites having different fixed carbon content were carried out non-isothermally up to 1200oC in Ar atmosphere using thermogravimetric anlyser (TGA). Quadruple mass spectroscopy (QMS) was also adopted to measure the CO, CO2 concentrations in the off gases resulted during reduction process. The effect of volatile matter on the reduction of iron oxide was intensively studied. The different phases developed in the reduced product were identified by X-ray diffraction (XRD). The reduction of composites was found to proceed in a stepwise manner (Fe2O3?Fe3O4?FexO?Fe).

Jan 1, 2015

By D. H. Yardley

Diversion of the American Falls of Niagara to permit investigation of ways and means to stabilize the falls while retaining or improving its natrual attractiveness is the geoengineering work that has received greatest public attention this year. The falls are re- treating slowly as rock falls occur while talus de- posits at the base have increased in size. One of the noteworthy questions is whether the talus should be removed-i.e. is it providing support to the base, and so what will happen if it is removed? Certainly the appearance would be improved if the talus were taken away. Geoengineering studies involve mapping of joints, stress measurements, core work and rock sampling and testing, Present work will provide data and interpretation for design of a long term stabilization system, Once basic information is obtained, water will be returned to the normal channel until such time as the detailed design is decided upon. The falls will then be diverted a second time while necessary work is performed. A number of site-environmental studies were carried out for the location of nuclear power plants. These projects involve geology, foundation engineering, hydrology, seismology, meteorlogy, marine geology (in some cases), rock mechanics and occasionally blast monitoring. In one case (investigated by Dames & Moore) the site area was underlain by caverns in limestones at shallow depths but with no surface expression. The geotechnical problems consisted of determining proper spacing of drill holes to locate caverns. Spacing was dependent on the smallest size of cavity that could constitute a support-stability problem for the plant. The finite element method of analysis was used to determine stress conditions around cavities of various size and depths, to assist in determining critical parameters.

Jan 1, 1970

By L. W. Ashton

Geochemical exploration guidelines were developed from a study of 460 rock chip samples collected at nine disseminated gold deposits in Nevada. Obtaining high grade Au samples is difficult because gold content is extremely variable, even over 8 m (25 ft) distances. For reconnaissance sampling, pathfinder elements are reliable indicators with threshold values of 100 ppm As, 1 ppm Hg, and 50 ppm Sb. Arsenic is the most reliable of the three elements, being significantly enriched in all deposits. If the pathfinder threshold levels are reached with low Au content, more samples should be collected. Successful disseminated gold exploration requires large numbers of samples.

Jan 1, 1990

By William A. Dupree, Mark J. Schultz, William J. Francart

Maintaining intake escapeways clear of contaminants from mine fires has been an issue for many years. Removing fire sources from these entries reduces the risk of contamination greatly. In recent years, concerns have been raised related to contamination of the intake escapeways by leakage when fires occur in adjacent airways. This paper discusses measured leakage rates for multiple stoppings at various pressure drops across stopping lines in a number of actual coal mines. Also addressed are methods for reducing the contamination risks for the intake escapeways, considering the ventilation system employed. The Effects of Air Leakage The effects of air leakage through ventilation controls has been well documented. While normal leakage is expected through stoppings, overcasts and other structures, abnormally high leakage results in an inefficient ventilation system and can increase operational costs for a mine. In addition, excessive leakage results in less control over mine ventilation airsplits. This may compromise the isolation of mine escapeways, and allow adjacent entries to be rapidly contaminated by products of combustion in the event of a mine fire. A study was conducted at ten mines in which air pressure and quantity measurements were taken near the active sections. The method used to construct the ventilation controls to separate airways was also noted. Stopping Construction Table 1 shows the type of stopping construction commonly used in the 10 mines included in this study. Main entry stoppings were normally built with mortared joints (wet stacked) with sealant applied to the high pressure side of the stopping. In most cases the entire face of the stoppings were sealed. In one case only the joints between blocks were sealed but the perimeters were sealed in all cases. Some mines also sealed the low pressure side of the stopping. Solid blocks were normally used for main entry construction and hollow blocks were sometimes used for longwall panel development. [ ]

Jan 1, 1993

By R. K. Buhr, H. Thresh, M. Bergeron, F. Weinberg

The microsegregation of nickel and chromium in directionally solidified AISI 4340 steel castings has been measured using electron probe microanalysis. Minimum concentrations were observed to occur at the center of the dendrite stalks, as reported previously. However, the position of the maximum concentrations could not be determined from the dendrite configuration. An etching technique has been developed which shows the position of maximum concentration. Measurements were made of the distribution of nickel and chromium in the dendritic structure. The ratio of maximum to minimum concentration was determined as a function of primary dendrite arm spacing for both as-cast and partially homogenized materials. The results are compared with observations reported in the literatuve. A S part of an investigation of solute segregation in directionally solidified AISI 4340 steel casting, electron probe microanalysis was used to measure the distribution of nickel and chromium in the dendritically segregated material. This complemented the observations on the segregation of radioactive phosphorus obtained by autoradiographic techniques in the same castings.' Kattamis and I?lemings2 have reported similar measurements, using electron probe microanalysis, on dendritically segregated AISI 4340 steels. They found minimum solute concentrations occurred at the center of dendrites, maximum concentrations occurred in the center of interdendritic regions, for symmetrically oriented dendrites, and a regular variation of concentration within dendrite arms. The ratio of maximum to minimum concentration was found to be essentially independent of position in the castings, except near the chill surface where it was somewhat higher. Assuming complete diffusion in the liquid and no diffusion in the solid during freezing, they considered that isoconcentration curves in the steel were homothetic. As a result, isoconcentration curves of the various elements, contour surfaces of dendrites produced by isothermal-transformation studies, and the contour of the solid-liquid interface would all be similar, and could be superimposed by a uniform expansion or contraction of the contours. Preliminary results of the present investigation suggested that isoconcentration curves were not homothetic. It was also evident that points of maximum concentration could not be predicted from the dendrite configuration. Since the ratio of maximum to minimum concentration appeared to be an important parameter in defining the overall segregation in a casting, other techniques for determining the point of maximum concentration were investigated. In addition the overall solute distribution associated with the dendritic structure was examined for both nickel and chromium, and the consistency of the distribution for neighboring dendrites was determined. METHOD Fifty-pound heats of AISI 4340 steel were cast in a manner similar to that used by Flemings et al3 with a water-cooled copper base plate and exothermic sides and top. The nominal composition of the material was C, 0.41 pct; Mn, 0.66; Si, 0.35; S, 0.012; P, 0.010; Ni, 1.88; Cr, 0.95; Mo, 0.28. The steel solidified directionally from the chill surface, with a dendritic structure which increased in dendrite arm spacing with increased distance from the chill. Results of the general investigation of the cast structure and segregation of radioactive phosphorus in these castings have been reported elsewhere.' For the present measurements, sections were cut from the casting at several distances from the chill surface. The sections were subsequently heat-treated, mounted, and then polished on a plane perpendicular to the general freezing direction of the casting. Electron probe microanalysis was carried out with the JEOL-JXA3 microprobe using a voltage of 25 kev and beam current of 0.15 µa. The take-off angle is 22 deg. Quartz crystals were used in the spectrometers and measurements made for Ka radiation from both nickel and chromium simultaneously. A thin layer of carbon was deposited on all specimen surfaces prior to examination in the microprobe. Early measurements were made on polished surfaces, with indentation marks produced by a hardness tester to indicate the area of interest. It was found desirable to use etched surfaces, as opposed to polished surfaces, to reduce sample preparation time and more readily relate the microprobe scan to the structure. To determine if this could be done, without introducing significant errors, a series of measurements were made on polished and etched surfaces of the same specimen. Both polished and etched surfaces produced similar results within normal scatter as shown in the observations. Subsequent measurements were then made on etched surfaces. Measurements with the microprobe analyzer were made by point counting, for periods of 100 sec, at 10-µ intervals. Ten-second counts were made on pure nickel and chromium standards, incorporated in the specimen mount before and after each set of measurements. The results were adjusted for background, then corrected for dead time using the expression:

Jan 1, 1969

By Theodore Marvin

USE of airplanes to facilitate mining and petroleum operations has definitely left the "doubting Thomas" stage. As a matter of fact, front pages no longer record the novelty of this efficient arm of the mineral industry. We are now down to the facts basis. The recent aviation issue of Engineering and Mining Journal added - to our fund of knowledge on applications which the A.I.M.E. Aviation Committee is extensively adding to through its world-wide compilation of specific data. Another indication of the advance of flying in our. industries is the addition of regular aviation specialists to the staffs of various mining and petroleum companies, who function in the organization the same as do the metal

Jan 1, 1936

By S. Kashani-Nejad

The kinetics of the thermal decomposition of samples of Mg2(OH)3Cl.2H2O that were obtained by a novel leaching technique applied to a commercial magnesium electrolysis feed were investigated under ambient atmosphere. Thermogravimetric (TG) Analysis showed that decomposition of Mg2(OH)3Cl.2H2O exhibited a single intermediate stage wherein crystalline water was lost at roughly 108 °C. Conversion of the resulting Mg2(OH)3Cl to MgO, HCl and 1120 occurred at temperatures above 398 °C. Thermal decomposition of anhydrous Mg2(OH)3Cl was seen to be consist of two stages. Both stages exhibit first order kinetics with respect to the weight percent of Mg2(OH)3Cl remaining in the sample. However, the rates of decomposition in the two stages were significantly different. Detailed analysis of the kinetic data suggested that the rate of decomposition of Mg2(OH)3C1 was controlled by the rate of removal of the gases released. The change in decomposition rate during the course of the experiments was explained by HCI being released in stage 1 and followed by release of H2O in stage 2.

Jan 1, 2004

By Arthur F. Johnson

Plant sites for the light metal industry must be located where ample low cost power is available. In the first half of the century hydroelectric development was the only source of this power-now the best sites have been exploited and those remaining do not promise enough water to permit year-round capacity power plant operation. In searching for economic plant sites engineers have concentrated on locations with vast water power potential. Olin Mathieson Chemical Corp. has been studying the economics of developing water power to make aluminum. However natural gas, lignite, and even atomic energy have also been considered as possible power sources for aluminum production. Economic studies have given consideration not merely to investment and production costs, but to total costs of delivering fabricated products to the market center of the U. S. When delivered costs are considered and when full account is taken of the newest techniques of mining bituminous coal and utilizing it to make electric power, one arrives at the inescapable conclusion that coal has emerged as the economic answer to American aluminum production.

Jan 4, 1955

By Thomas S. Lovering

Hot springs, geysers, steam-emanating fumaroles- these creatures of nature were until recently little more than geological curiosities, but today they are exciting the interest of engineers around the world for it has been shown that such hyperthermal areas can be profitably harnessed by man to provide heat and power for his communities. Although water from hot springs was used centuries ago to heat some Korean dwellings, is being used today by one-third of Iceland's population for similar purposes, and is finding industrial applications in New Zealand and elsewhere, the most dramatic use of geothermal energy has been its conversion into electricity. The largest installation at the present time is that at Larderello, Italy, where the Count of Larderello began to experiment in the production of electricity from geothermal steam in 1904. Eight years later after a quarrel with the local power company, the Count installed his first steam turbine, a unit of 250 kw capacity.

Jan 9, 1965

By E. C. Roper

Landusky Mining, Inc. and Zortman Mining, Inc. are two registered Montana Corporations wholly owned by Pegasus Gold, Ltd. of Vancouver, B.C. The Zortman and Landusky Mines are located in the Little Rockies District of central Montana. The Zortman-Landusky mines produced 2,100 kg gold in 1982. A total of 3,250,000 t of ore per year are mined during the period March 1, to September 15, at an average grade of 1.04 gm/t (0.03 oz/t) gold and 13.4 gm/t (0.385 oz/t) silver at a cutoff grade of 0.35 grams of gold/ton (0.01 oz of Au/t) of ore. The stripping ratio during 1983 is anticipated to be 0.75/1 waste to ore. Combined average plant capacity of the two Merrill-Crowe plants is 9,840 lpm (2,600 gpm). The combined heap spray capacity of the two plants approaches 18,900 lpm (5,000 gpm). The mine employs approximately 200 people, about half of these work for the mining companies and the other half for the mining contractor, N. A. Degerstrom of Spokane, Washington. Net profit in 1982 for Zortman and Landusky Mining, Inc. approximated $4,900,000 at an average gold price of $11.40/gm.

Jan 1, 1983

"The National Mining Hall of Fame and Museum (NMHFM) announced the class of 2019 National Mining Hall of Fame inductees. This year’s inductees, selected by the National Mining Hall of Fame’s Board of Governors, represent exceptional financial acumen in assembling several operations that formed the basis of a successful American mining company; conception and development of equipment which contributed to improved efficiency and mine safety; and unrelenting advocacy for the U.S. mining industry and its workers. These individuals, selected for being determined, forward-thinking innovators, doers and leaders have propelled the industry toward vastly improved safety and social responsibility.The Prazen Living Legend of Mining Award, named for renowned mining artist Gary Prazen, will also be presented at the ceremony. This award recognizes an individual or organization for significant and sustained commitment to educating the public about the relationship of mining to our everyday lives through educational materials, programming, and outreach.2019 National Mining Hall of Fame inducteesFrank Calandra, Jr. has devoted more than 50 years to the mining industry and he is an icon in ground control technology for the mining, tunneling and civil construction industries.From the ground up, his passion, sweat equity and shrewd business acumen have grown Frank Calandra, Inc. (FCI) and Jennmar from a single plant in Pennsylvania to a world-class enterprise with 25 plants employing thousands globally. As evidenced by Calandra’s more than 20 patents on ground control devices (not to mention the additional 80 patents his companies hold), his innovation and commitment to safety have made underground mining safer and more efficient. In the late 1970s and early 1980s, Calandra was instrumental in upgrading American Society for Testing and Materials (ASTM) standards in roof control for both state and federal regulations. Through his work with industry associations such as the National Mining Association, National Coal Council and Center for Energy and Economic Development, among others, Calandra has contributed his time, expertise and financial support to ensure a balanced political and regulatory climate for mining. Calandra is an inductee of the West Virginia Coal Hall of Fame."

Aug 1, 2019

The following is an incomplete list of members and guests who called at Institute headquarters during the period June 10, 1919, to July 10, 1919. Anvil A. Anderson, Rapid City, S. D. Roy N. McBride, U. S. Army. R. Hay Anderson, Mexico City, Mex. R. S. McIntyre, Berkeley, Calif. W. A. Barnes, San Francisco, Calif. H. R. Maier, Brooklyn, N. Y. Bennett R. Bates, Denver, Colo. Wm. D. Mainwaring, Philadelphia, Pa. Harlan H. Bradt, Duluth, Minn. Wm. E. Milligan, Chrome, N. J. H. Brings, San Francisco, Calif. Willard S. Morse, Tacoma, Wash. Robert S. Burg, Ocean Park, Calif. Arthur Notman, Bisbee, Ariz. D. W. Butner, Congo Belge, Africa. P. Nugue, Chalon Sr. Saone, France. George A. Camphuis, El Paso, Tex. George A. Packard, Boston, Mass. Fred Canan, Denver, Colo. C. L. Petzel, New York City. Walter H. Coleman, Prescott, Ariz. V. Porreaud, Paris, France. Fred Crabtree, Pittsburgh, Pa. Fred S. Porter, Seattle, Wash. Ross E. Douglas, Rancagua, Chile. R. W. Prouty, Morenci, Ariz. F. A. Downes, Golden, Colo. Charles E. Prior, Brooklyn, N. Y. W. G. Eberhardt, Tucson, Ariz. Louis Ravicz, Minneapolis, Minn. Charles H. Fulton, Cleveland, Ohio. Wm. Reed, El Oro, Mexico. Wm. R. Grunow, New York City. E. J. Ristedt, Globe, Ariz. Orr R. Hamilton, Lansing, Mich. A. M. Rodgers, Middletown, N. Y. T. N. Havlin, St. Louis, Mo. J. C. Scoles, Salt Lake City, Utah. G. M. Henderson, Weston, Mass. C. E. Siebenthal, Washington, D. C.

Jan 8, 1919

By L. "Andy" Anderson, Stephen N. Short, James E. Friant

Since the introduction of "boxhole" drilling in South Africa in 1973, the concept of a blind raise, drilled upward from below, has become an accepted mining practice. A combination machine, capable of constructing raises to a mining level below, or blind raising upward from a single setup position adds a further dimension in versatility. A machine with these dual operating modes was designated by The Robbins Company as the 53R and was introduced into the Western Deep Level Mines, South Africa in 1984. The unit is powerful (200 hp) and compact (18,000 lbs., in a 10 ft x 4 ft 5 inch x 4 ft 6 inch package). This paper describes the design considerations for the new machine, provides field data from early trials, and looks briefly at its overall market and potential.

Jan 1, 1985

By P Gilroy

In recent technical investigations that were triggered from ore for rail shortfalls at Yandi, BHP Iron ore has identified a gap in resource knowledge relating to geo-metallurgical characteristics that predict materials handling performance and throughput. Within these investigations BHP has learnt that this lack of resource knowledge has translated to a lack of predictability associated with mine planning inputs which has resulted in poor compliance to plan and deviation management practices. A business value chain was developed in an attempt to identify the best possible solution to unlock this resource knowledge in the short, medium and long term planning horizons. A fast fail approach was taken with the implementation of hyperspectral blasthole analysis, which was chosen to deliver the best possible value driver for the asset. This report will detail the Yandi journey in expanding the hyperspectral and geo-metallurgical value chain, unlocking resource knowledge along the way. CITATION: Gilroy, P, 2018. Development of an empirical geo-metallurgical model that unlocks value of the mineral resources at Yandi Mine, in Proceedings Complex Orebodies Conference 2018, pp 85–87 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 21, 2018

By J. D. Morgan

In the first half of the year, lessening of cold war tensions was welcome. But Iraq's invasion of Kuwait in the second half led to the Persian Gulf War in January and February 1991. This caused an oil shock that dampened the economy. So the US gross national product rose only 0.9% to $5,463 billion (US billion = 109). The buildup of military forces in the Persian Gulf area focused greater attention not only on petroleum but also on other strategic materials. The Department of Defense continued to review stockpile goals and to upgrade several mineral materials. In addition, the Bureau of Mines continued to maintain the standby Emergency Minerals Administration. The Defense Production Act, which authorizes priorities, alloca¬tions and supply expansion, lapsed on Oct. 20. So the Selective Service Act of 1967 became the authority for assuring that orders of the armed forces and defense atomic-energy programs were given priority treatment. Consumer demand strongly affects mining worldwide. US citizens carry significant debt, and large stocks of housing and consumer goods are already in place. Some 250 million persons have 188 million licensed motor vehicles and 100 million dwelling units. Consequently, new car production fell 11 %, to 6.1 million units. Truck and bus production fell 8%, to 3.7 million units and new private housing starts fell 13% to 1.2 million units.

Jan 1, 1991

By R. G. Sandberg

The Bureau of Mines investigated a hydrometallurgical procedure to recover gold, silver, and byproduct lead from a complex lead-zinc sulfide ore. A ferric chloride (FeCI3) preleach, at 40° C in 6 h, extracted about 50 pct of the zinc and formed insoluble silver and lead chlorides. Subsequent acid thiourea leaching, for 1 to 3 h at 40° C, extracted about 85 pct of the gold and silver. Lead chloride was solubilized from the remaining residue with NaCI brine solution at 55° C in 1 h. Lead metal was recovered from the brine solution in an electrolytic cell with an anion perms elective membrane at a current efficiency of 95 pct and current density of 100 A/m2. Spent FeCl3 leach solution was reoxidized in the anode compartment at a current efficiency between 75 and 95 pct.

Jan 1, 1986

By Gordon Bath

During the summer of 1946, the Division of Geophysical Exploration of the U.S. Bureau of Mines established several primary magnetic base stations near important iron-producing districts in Minnesota, Michigan, and Wisconsin. Stations were located in groups of four to six in six separate base-station areas, and each position was marked with a concrete monument. Differences in magnetic intensity between stations in these areas, as well as the difference between each area and a magnetic datum at the magnetic observatory of the Coast and Geologic Survey at Cheltenham, Md., were measured with a modified Askania magnetometer. Measurements also were made with a Hotchkiss superdip to study the usefulness of the stations for the calibration of instruments of this type. The work was planned and supervised by F. W. Lee, chief of the Division of Geophysical Exploration, and Edward F. Fitzhugh, Jr., chief of the Minneapolis Division of the Bureau of Mines. Special mention is due Harold B. Ewoldt, Bureau of Mines engineer, for his assistance in the field work, especially in locating and establishing monuments. Special mention also is due Clyde L. Holmberg, of the Bureau of Mines, for the magnetic measurements made with the Hotchkiss superdip. Helpful suggestions were received in the field from H. L. James, of the U. S. Geological Survey. Acknowledgment is made of the cooperation of Stephen Royce, Irving E. Beckwith, Arthur Johnson, and Josiah Royce of Pickands, Mather & Co., and A. E. Matson, of Butler Bros. The U. S. Coast and Geodetic Survey furnished daily magnetograms from the Cheltenham Magnetic Observatory as well as calibration equipment and values of absolute magnetic intensity. Short-term forecasts of ionospheric conditions were obtained from the National Bureau of Standards.

Jan 1, 1951

By Henry Stoch

It?s a green, green world ? Public concern about the impact of human activities on the environment and the roles that businesses play in that impact is rising. What?s happened in the last few months? ? Recent news: ? British Columbia announces carbon tax in 2008 budget ? Federal Court ruling stalls oil sands approvals due to a lack of consideration of GHG implications ? US Energy Independence and Security Act could limit government procurement of oil sands-derived fuels ? Western Climate Initiative (WCI) suggests a ?first seller? approach for regulating generators outside WCI jurisdictions ? Implications ? A cost for carbon has arrived ? The lack of a GHG strategy can have a material impact on your business ? Regulations in other jurisdictions could affect your organization

May 1, 2008

By L. B. Underwood, C. J. Distefano

NORAD, when completed, will be housed in large chambers excavated out of the granite beneath the Cheyenne Mountain near Colorado Springs. A room and pillar layout for the chamber excavation was selected and executed. Many complex problems arose in designing a rock bolt system; this paper includes discussions on: rock strengthening following excavation, excavation and ground support problems, orienting rock bolts with respect to jointing systems, conducting pull tests, four-way chamber intersection problems, the need for grouting rock bolts, and loss of tension and permanency of anchorage in a rock bolt system. In the event of a sudden nuclear attack upon the United States, it is imperative that vital command and control centers have a high probability of survival. One such vital facility is the North American Air Defense Command Combat Operations Center at Colorado Springs, Colo. Known briefly as NORAD, this installation when completed will be housed in large chambers excavated out of granite beneath the eastern slope of Cheyenne Mountain (Fig. 1). The NORAD COC, a U.S. Air Force sponsored project, will serve as the primary collection and evaluation center for data concerning unknown aircraft, missiles, or space vehicles, which might bring destruction to North America. The data will be fed into high-speed computers and electronic equipment from outpost sources: radar, ballistic missile early warning stations and picket ships throughout the world. Electronically controlled display boards will make it possible to evaluate the tracking data instantaneously and to take appropriate defensive action.'

Jan 1, 1968

By C. B. Alcock, L. I. Cheng

By the use of radiochemical methods for the study of the gas-liquid equilibria at low temperature, and for the determination of the sulfur contents of metal beads which had been equilibrated with H2S/H2 mixtures of known sulfur potential, it has been possible to obtain the liquid solubility and the free energy of solution of sulfur in liquid tin and lead at temperatures between 500°and 680°C. THE gas-liquid equilibrium method has proved in the past to be most successful in the determination of the thermodynamic behavior of dilute solutions of sulfur in liquid metals.1,2 One of the basic requirements for success with this method is that the volatility of both the metal and its lowest sulfide should be small, otherwise sulfide will be deposited at the cool end of the furnace, where it may react with the outgoing gases to form either sulfur-rich lowest sulfide or higher sulfides. The resultant value of the apparent equilibrium constant will then be lower than the correct one. This argument applies even at sulfur potentials below that in equilibrium with a separate condensed phase of the lowest sulfide at the reaction temperature, T. The mass of sulfide which is deposited at the cold end of the furnace, and hence the extent to which further reaction occurs with the outgoing gases, depends on the time taken for equilibrium to be reached between metal and gas. Since this will depend principally on the bulk of the metal phase which is used, one should clearly attempt to uie as small metal samples as possible. These considerations are important in the study of dilute solutions of sulfur dissolved in liquid tin and lead which both have moderately high vapor pressures as metals and form volatile sulfides. The limit on the size of the metal samples which may be used is set chiefly by the difficulties of analysis for very small amounts of sulfur. The oxygen or carbon dioxide combustion method, followed by iodimetric determination of the sulfur dioxide which is formed,has been found to be successful for the determination of small amounts of sulfur in copper, iron, cobalt and nickel.4 This method was unsatisfactory for sulfur dissolved in tin and lead, mainly because the sulfur dioxide was to some extent absorbed by the copious tin or lead oxide deposits which were formed on the walls of the combustion tube. Furthermore some of the sulfur was found to segregate on the surface of the beads as flaky sulfide crystals which would easily be lost in the transfer of a bead from a boat in the gas equilibration apparatus to one in the combustion apparatus. Oxidation in aqueous media to sulfate ion followed by precipitation as barium sulfate was, therefore, adopted as the analytical procedure. The gas-metal equilibrium experiments were all carried out with radioactive sulfur and thus the analysis involved the counting of barium radiosulfate. Furthermore the use of the radioisotope meant that the approach to the gas-metal equilibrium could be followed continuously by gas counting.' The metal beads were held separately in glass crucibles during equilibration and were transferred from the furnace to the beaker for dissolution in nitric acid still in the crucibles, and thus the possibility of sulfur loss by detachment of the sulfide segregates was eliminated. The temperature range of this investigation was 500° to 680°C. EXPERIMENTAL APPARATUS AND METHOD The apparatus consisted of two furnaces placed in series in a gas recirculation system, Fig. 1. One furnace F1, which was vertical was used to heat the alumina crucible, A, holding six metal beads in separate glass crucibles. The beads weighed between 300 and 700 mg each. The crucible assembly was introduced and removed from the furnace mechanically under a stream of oxygen-free argon. The other furnace, F2, was horizontal and was used to heat a cobalt Co9S8 mixture, held in an alumina boat, and made with radiosulfur containing about 1/2 millicurie per g of sulphur. This mixture, which was finely powdered, was used as a source of known H2S/H2 mixtures6 for a given furnace temperature. The recirculation system also contained a gas re-circulation pump (P), an end window Geiger-Miiller counter (N)—placed downstream of F1 so as to monitor the H2S pressure in the gas leaving this furnace— a sample volume for chemical analysis of the gas phase (G), gas drying tubes (D), filling taps and other standard ancillary equipment. The gas sampling volume was principally used in the cali-

Jan 1, 1962