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By M. J. Ankeny, J. J. Forbes

"One of the main functions of the U. S. Bureau of Mines, as authorized by Congress, is to investigate safety and health conditions, to disseminate information regarding safe and unsafe practices in mining, and to aid in improving safety and health conditions of mining communities and in promoting the welfare of the miner. Among several methods of reaching the miner and interesting him in safety work, perhaps the most effective is through the 11 mine safety stations and 11 railroad cars known as mine rescue, or more correctly, mine safety cars.Frequently, the Bureau of Mines receives requests for information regarding the purpose, equipment, personnel, and construction of its safety cars used in the field service. It is the intention of this circular to present to the mining public in particular, and to the public in general, some definite information regarding these safety cars and their functions.The cars are operated throughout the mining fields of the United States and are headquartered as follows (see fig. 1): Car 1, Reno, Nev.; Car 2, Raton, N. M.; Car 3, Pittsburgh, Pa.; Car 4, Terre Haute, Ind.; Car 5, Pineville, Ky.; Car 6, Pittsburg, Kans.; Car 7, Huntington, W. Va.; Car 8, Duluth, Minn.; Car 9, Butte, Mont.; Car 10, Des Moines, Iowa; Car 11, Anchorage, Alaska.One of the most important purposes of the U. S. Bureau of Mines safety cars is to render service at mine fires and explosions where human life is endangered. State mine inspectors and other interested persons are supplied with itineraries of the car operating in their districts from time to time, so that they may know at all times where the car can be found in case of emergency. When these disasters occur the car may be reached direct or through its field headquarters, and upon receiving word of a mine disaster, or request for assistance, it immediately proceeds to the scene of trouble. Frequently a special locomotive is supplied by the railroads and in many instances the movement of the car is given the right of way over all other railway traffic. Upon reaching the destination, the facilities and personnel of the car are immediately available for rescue and recovery operations.Following most mine disasters a thorough investigation is made by engineers of the Bureau of Mines, and a confidential report is submitted to the operator. The information gained in this manner from a large number of mine fires and explosions, together with the knowledge gained from the experimental work carried on at the Experimental mine of the bureau at Bruceton, Pa., serves as a basis upon which the bureau is able to recommend preventive measures whereby similar occurrences may be averted. The bureau car is often used as headquarters for the investigating engineer when such an examination is being made."

Mar 1, 1931

By I. Liebman

The Bureau of Mines conducted experiments on coal dust explosion suppression. The investigation took place on a beltway in the double-entry of the Bureau's Experimental Mine. Using conditions that simulate those in a working mine, the investigation showed that a coal dust explosion can be readily initiated in a conveyor belt entry. Also, the explosion can spread into adjacent entries through opened crosscuts (stopping destroyed by explosion) to propagate for long distances even though the adjacent entries are rock dusted in compliance with regulations. Passive water barriers (water-filled tubs) were found to be effective in suppressing explosions on a beltway; however, barrier efficiency was reduced by opened crosscuts. The study indicated that the beltway barrier should be the distributed type consisting of continuous rows of water-filled tubs covering long distances along the entry. A plan is outlined for the installation of a water barrier system in a working coal mine for the protection of a beltway.

Jan 1, 1981

By H. R. Peterson, G. J. Lipovetz, W. F. McDermott

One of the major improvements in ore grinding economics in North America has been the introduction of autogenous grinding. Pickands Mather & Co. has been active in the development of autogenous grinding since 1957. This early work led to the application of autogenous grinding to the Wabush mines ore in 1965, with the installation of six 24 ft diam by 8 ft long, 1750-hp mills. Development work recently completed in 1971 on another ore has led to the decision to install five 36 x 15-ft, 12,000-hp mills when this project goes ahead. Between these two decisions lies a tremendous amount of research, development and application of autogenous grinding to a variety of ores. The Pickands Mather Metallurgical and Research Laboratory in Hibbing, Minn., has tested ores from 9 different deposits in its pi- lot plant facility. Some of these deposits have as much difference within their own ore types as there is between the various deposits. Therefore, it is safe to say that over twenty different ore types have been tested and flowsheets developed for commercial applications. Of the nine projects, three are in operation. These are Wabush mines in Labrador, Canada,' Savage River mines in Tasmania,' and The Griffith mine in Red Lake, Ont., Canada.'

Jan 11, 1972

By M. G. Karfakis, K. P. Chong

Determination of fracture toughness using the semi-circular specimen, the chevron edge notch round specimen, the short rod specimen and the cylindrical burst specimen, are critically reviewed. These methods, among all, are the most applicable for fracture toughness determination of rocks. They require minimum machining. Samples are small, and testing procedures are simple. They have a sound analytical basis and allow the fracture toughness to be determined without measurement of fracture length.

Jan 1, 1986

By F. Fraas, J. E. Conley

"The problem of recovering potash from the mineral polyhalite (K2SO4.MgSO4.2CaSO4.2H2O), occurring in large quantities in the salt beds of Texas and New Mexico, has been under investigation at the Nonmetallic Minerals Experiment Station of the U. S. Bureau of Mines continuously since 1928. Most of the results previously obtained have been published in technical journals and in a series of Bureau of Mines Reports of Investigations.The experiments described in the present report were performed to ascertain whether a continuous countercurrent extraction of calcined polyhalite by hot water would yield satisfactory recoveries and concentrations of sium sulphate in the top liquor. Previous investigation by Storch 4 had shown that the rate of solution of uncalcined polyhalite was too slow to be of value in an industrial process, and Storch and Clarke 5 had demonstrated that calcination of the polyhalite greatly, accelerated the rate of solution in hot water, allowing most of the potassium sulphate to be readily extracted."

Sep 1, 1933

By Jury P. Nazarov

"At present the traditional study of crystal lattices of nmerials in a topic “flota tion mineralogy ” is used up. The present investigation is development of the a sclsical approaches to t he analy sis of ideal crystal lattices and f ormation on the basic obtained results of consultation, having practical chara cter.The strategy of develop ment floatation reagents i s offered, which basic pr inciple – complementary assembling m olecules forming surface co mpounds so thatth e steric charact eristic of the “visitor "" (of a polar gro up of molecule SAS) corresponded to the st er ic requirements of the ""o wner"" (elementary cell of a mineral), or coincided inter molecular cavities). In itsh case process of for mation of surface com pounds ca n be considered(a first approximation) as a realization of a principle of the design er "" LEGO "".The approach, which basic idea consi deration actioonf reactant ions and ions of ele mentary cell as three-di mensional objects is developed. And at suchp paroach the laws of a ster eometry - laws describin g spatial effect s are applicable. Thus it is possible toconsider a miner al surface as a mat r ix - basis for formation of the requirem ents to polar group of a molleec cuollector, and or (it is possible) depressant. As a whole approach represents a generalized principle double com plementation, enveloping both power, and geometric asp ects (concept ""lock "" and “key "" - spatial conform ity. Figure 7 (left). Fragment of a crystal lat tice of ap atite. Oleic acid ions interact on ly with th e calcium cations locate d on a long axi s of an elementary c ell. Magenta colour represe nts the calciu m cations, which are n ot particip atin g in interactio n, as th e degree of screening by ions neighbours exceeds 1.Figure 2. (right)The illustration of space complementary. “Afterbuilding” an elementary cell of apatite (radical PO4) related molecules of the visitor – alkyl phosphate (polar group PO4). Cations of calcium are not shown."

Jan 1, 2003

By Clarence O. Babcock

Model pillars of limestone, marble, sandstone, and granite with length-to-diameter (L/D) ratios of 3, 2, 1, 0.5, and 0.25 (0.286 for granite) were tested to failure in axial compression to determine to what extent an increase in end constraint increased compressive strength. Adjustable steel rings, mechanically tightened about the ends of test specimens to create a radial prestress of 3,000 or 5,000 psi prior to the application of axial load, increased end constraint more than was possible in previous tests using solid steel rings. (Solid rings, epoxy-bonded to the ends of dogbone specimens, increased compressive strength compared with that of straight specimens without ring constraint.) During the loading cycle, additional end constraint was produced by lateral expansion of the specimens against the rings. The effect of the end constraint was to increase the compressive strength 55 to 58 percent for the shorter pillars of dogbone shape compared with the compressive strength of straight pillars with the same L/D ratios without ring constraint. Most pillars with L/D ratios of less than 2 were made stronger by end constraint. Pillars with an L/D ratio of 3 did not benefit significantly from end constraint. When the results from compression testing of straight specimens of rock in the laboratory are used to design mine pillars in situ, the pillars will be larger than necessary if the horizontal compressive stress is several thousand pounds per square inch greater than that resulting from the weight of the overlying rock alone. The L/D ratio can be increased by a factor of 1.76 for ratios in the range 0.25 to 3 and still provide the same compressive strength. The safety factor applied with straight specimen test results should also be acceptable for use with constrained pillar test results.

Jan 1, 1969

By Michael R. Cartwright

The Gold Acres outcrop was located by Lee Lakin in 1922, according to Mr. H. W. Treweek. There was no activity, however, until 1935, when prospect drifts and pits penetrated the deposit. It was then drilled by the Willow Creek Mining Company. Beginning in the late 1930s and continuing to the late 1940s more than 150 churn drill holes were drilled in the Gold Acres area. From this drilling came what is now known as the London Extension pit. Only oxidized ore amenable to cyanide vat leaching was mined during this time. Our records indicated that this period of mining removed some 1.4 Mt (1.5 million st) of ore at an average grade of 0.006 kg/ t (0.2 oz per st). Union Pacific and Newmont Mining Company worked in the area prior to acquisition by the Cortez Joint Venture. Union Pacific drilled a number of core holes in the area. The unoxidized nature of the ore, small tonnage, and low grade undoubtedly prevented mining at this time. From these indications of mineralization shown by previous companies, the Cortez Joint Venture developed and mined 2 Mt (2.4 million st) at 0.005 kg/t (0.15 oz per st) in the Gold Acres pit. This pit is located immediately southwest of the older London Extension pit. Cortez Gold Mines has continued to drill to the west and south of these pits along the downdip continuation of the former ore bodies. The downdip extension is unoxidized and more metallurgically difficult than the normal Carlin type ores, but, more than 2.4 Mt (2.7 million st) have been outlined. It depends now upon the gold price and milling costs to turn this mineralized area into an ore body. A possible lesson to be learned from this deposit is that continued mining success depends upon an ongoing adequately funded exploration-development-metallurgical research program. These three disciplines must always be present to locate the mineralization and to turn this mineralization into ore. [ ]

Jan 1, 1985

By Stanislaw Wasolewski

Computerized systems for ventilation parameters monitoring which are used in Polish coal mines provide the ventilation staff with a great number of measuring data. These data can be used to get knowledge about dynamic properties of ventilation process and disturbances affecting its state. This is necessary to create a reasonable concept of mine ventilation control system and make a practical application of such system. In the paper a method of ventilation process identification with the use of measuring data from monitoring system is described. Computer analysis of time series including statistical, correlation and frequency methods are applied to estimate dynamic properties of ventilation process and its disturbances. Using the Fast Fourier Transformation (FFT) algorithm the parameters of the process have been obtained which can be efectively used in a system for mine ventilation control.

Jan 1, 1991

By E. S. Lenker, H. J. Van Hook

A complete swies of solid solutions has been found between the compounds InAs and GaAs Below the solidus. The melting relations determined by differential thermal and static quenching technzques, indicate that the liquidus and solidus are of the simple ascendant type. No evidence of unmixing of the homogeneous solid solutions was observed at sub-solidus temperatures. A quenching method for locnting the solidus, using X-ray diffraction techniques, is described in some detail. THE semi-conducting properties of compounds formed by various combinations of the less familiar intermetallic elements have created an increasing interest in the phase relations in systems involving these elements. The complete phase diagram of such a system, containing a compound of special interest, will often provide information as to the most favorable conditions for preparing large crystals from a melt, as well as specifying the temperature stability of the crystalline phase or phases produced. In view of the current importance of gallium arsenide in semiconductor research and of the structural similarities of indium arsenide, it was thought that the complete phase relations of the system InAs-GaAs should be investigated. Previous work on the system Ga-As by Koster and homa' and on In-As by Liu and peretti2 has shown that GaAs and InAs are the only compounds formed, having melting points of 1238° and 942°C, respectively. In a survey of various systems of elements from groups IIIb and Vb, spengler3 also re- Mines Ltd., for his continuing encouragement and for permission to publish the results of this work. ports complete miscibility of gallium, indium, and arsenic in the liquid state. In a partial investigation of the InAs-GaAs system, Woolley and smith4 found extensive solid solution throughout the alloy range. Their subsolidus work, however, was inconclusive at temperatures below 900" and they did not determine the liquidus relationships of the system. PRESENT INVESTIGATION The starting materials used were high-purity gallium, indium, and arsenic. The method of preparation of the compounds follows that devised by M. Shafer and is described in detail in a paper by Shafer and eiser.' The end-member compounds, GaAs and InAs, were first prepared by reaction of the elements in the desired proportions in evacuated silica glass vials. The vials were rotated in a furnace as the temperature was slowly raised to insure rapid and complete reaction at low temperatures. Thereafter the starting materials, GaAs and InAs, were melted by heating the sealed vials to 1300" and 1000°C, respectively; the vials in this case were filled as completely as possible to keep the vapor space small and thereby minimize the loss of arsenic to the vapor phase. Ten binary mixtures of these compounds were then prepared by reaction of the powdered material in the solid state just below solidus temperatures. At 900C preparations containing 3, 5, 8, 10, 25, 35, 50, and 75 mol pct GaAs were found to be single homogeneous phases, indicating a complete series of solid solutions between GaAs and InAs. Moreover, it was discovered that the homogeneity of any crystalline binary preparation could be very accurately checked by X-ray diffraction because of the large differences in unit cell dimensions of the end membe5s. The cubic lattice constant ofor GaAs is a = 5.652A and that of InAs is a = 6.061A

Jan 1, 1963

By Nathaniel Arbiter, Arthur F. Taggart

THE fact that the floatability of minerals with fatty-acid collectors changes as the pH of a pulp varies was utilized in the early days of flotation, when sulphuric acid was used with oleic acid to float sphalerite and galena from gangues which themselves float with fatty acids in alkaline pulps. Gaudin1 showed that this difference in floatability is a regular function of the extent of the change in pH. The present paper offers an explanation of the phenomenon, and on the basis thereof sets up recommendations for control of soap-flotation operations. EXPERIMENTAL Parallelism between floatability of a mineral in a given environment and its contact angle in that environment is so well established,' and the contact angle is so readily and rapidly measurable, that contact angles have been used throughout the experimental work to indicate relative floatability. Experiments comprised contact-angle measurements on a number of representative minerals and metals, and a variety of subsidiary tests designed to check and to amplify the contact-angle indications. Contact-angle measurements were made by the method described in detail by del Giudice.3 Sequence of procedure for determination of the points of Fig. I was: 1. Polish specimen. Most specimens yielded zero contact angle after polishing; a few showed a slight "cling." Cling is characteristic of specimens that pit on polishing; it is due to a residue of organic contamination, originally on the particle surface, which persists in the pits. The cling did not change total contact angle after conditioning, and is not, therefore, additive in the upper part of the curves of Fig. I. It may have broadened the bases of the curves for the affected minerals slightly. 2. The specimen was next conditioned in soap solution for 5 minutes. 3. The conditioned particle was transferred, under conditions that precluded surface drying, to an aqueous solution of the pH desired and contact angle determined. 4. The particle was thereupon transferred, again without surface drying, to water. The confirmatory tests will be described at the places pertinent in the argument. DISCUSSION OF RESULTS Gaudin and Vincent4 have shown that contact angles with heptoic acid as a collector decrease for a given specimen when the concentration of collector present falls below a certain value. A similar reduction in angle occurs with collector-conditioned particles that are visibly slime-coated, and varies roughly with the extent of coating. Since in the last case the reduction in angle is certainly due to reduction in the proportion of total conditioned mineral surface presented to the bubble, the authors believe that the same condition prevails in the first case cited, and that similar reduction in angle and floatability will occur whenever starvation quantities of collector are present, whether

Jan 1, 1943

By J. R. Frederick

Introduction In response to industry needs and requests, Joy Mining Machinery is aggressively evolving a "game changing" system of underground development mining machinery. This entry-development system (EDS) project is concentrated on providing clean, protected and ergonomic operator areas and a quantum leap in productivity. To meet these goals, a virtually continuous and automated mining system is needed. Operators must be able to efficiently and ergonomically perform required functions from a protected environment. Health-related issues, such as respirable dust and noise, must also be addressed. A new concept system of integrated face equipment, from the continuous miner to and including advancing the section belt and services, is needed. Phase I of the project was aimed at developing the bolting technology required. Through acquisition of Cram Australia and joint development efforts with Canyon Fuel Co., Joy now has this capability. The test platform, known as the Joy Multibolter, has successfully completed its trials at Canyon Fuel's SUFCo Mine (Fig. 1). These tests validated the bolting technology and operator protection and ergonomic issues. Phase II includes the development and testing of an integrated mining machine (IMM) capable of advancing a heading 1.5 m (5 ft) while simultaneously cutting a fullface width (single pass) and installing a complete bolt pattern. The IMM, unveiled at MINExpo 2000, incorporates the bolting technology of the Multibolter with automated full-face cutting. This machine was designed to meet Joy's stringent health, operator protection and 300m/d (1,000-ft/d) productivity goals. Phases III through V will include development of processes and integrated haulage, ventilation, power, material handling and section services advancing equipment. Processes and equipment developed will be designed for seamless integration into a complete entry development system. The focus of this paper is the new continuous miner (IMM) development, proposed testing and expectations for the EDS. The IMM is scheduled for commissioning and trials beginning in April 2001 at the SUFCo Mine. SUFCo Mine Canyon Fuel Co. is jointly owned by Arch Western Resources and the Itochu Corp. of Japan. It owns and operates three coal mines in Utah: the SUFCo Mine in Sevier County, the Skyline Mine in Carbon and Emery Counties and the Dougout Canyon Mine in Carbon County. Incorporating state-of-the-art-mining technology and advanced mine management practices, the SUFCo Mine is one of the most efficient underground coal mines in the world. The SUFCo Mine is located approximately 50-km (30 miles) northeast of Salina, UT, in the Wasatch Plateau portion of the Uinta coal basin. The mine property consists of 9,900 hm2 (24,470 acres) with approximately 118 Mt (130 million st) of recoverable reserves. Public utilities and industrial concerns purchase approximately 95% of the coal mined at SUFCo through short- or long-term contracts. Coal reserves are extracted by longwall mining, and the panels are developed using continuous miners. The longwall face at SUFCo Mine is 283-m (930-ft) wide, and the seam height ranges from 2.4 to 4 m (8 to 13 ft). The two development sections are in full operation using Joy 12CM12 continuous miners. Two super longwall panels, under development in the northeast portion of the lease block, are 4,270-m (14,000-ft) long with a 283-m (930-ft) wide longwall face. Each panel contains approximately 5.4 Mt (6 million st) of recoverable coal. SUFCo has been a world leader in productivity for a

Jan 1, 2003

By Ioannis Nicolaou

This paper demonstrates the method of approach for the optimization of such filters. This does not only incorporate the proven and simple recently developed equations for the calculation of the solids throughput, the residual moisture and gas throughput, but also introduces equations for the calculation of the specific product costs for both vacuum and hyperbaric filtration under consideration of the influences exerted by the filter compressor and a possible thermal drying. An easy-to-use method is offered which incorporates a special graphic representation concerning the plotting of the target parameters in dependence of the pressure difference with which the optimal process pressure difference can be established, independent of the specific cake permeability or product fineness. Finally, the optimization method is exemplarily demonstrated for a concrete application.

Jan 1, 1995

By D. J. Wall, T. D. Johnson, M. T. Parry, G. R. Heath

In coal-fired power stations coal is ground to a fine powder and then transported pneumatically at 25-30 m/s velocity to remote burners. Wear of the conveying pipework is a well recognised problem and traditional lining materials are Nihard and basalt. In many cases these are being replaced by alumina tiles in order to improve life and reduce the frequency of replacement. A programme of laboratory testing of candidate aluminas with AIO, contents between 85% and 99-5% has been undertaken and the results compared with field experience. This gives confidence in the erosion tests, which were designed to replicate most of the field conditions. However, it has not proved possible to draw correlations between the laboratory erosion rates and any of the materials’ bulk properties. SEM, TEM and microanalysis studies have therefore been made in order to look for microstructural aspects that could be influencing erosion rates and it has been shown that intercrystalline cohesion, the matrix phase and porosity appear to have most influence on wear performance. It is necessary to quantify these microstructural parameters if reliable erosion performance is to be obtained. This paper was read at the Institute of Ceramics Annual Convention at the University of Durham, April 1988.

Jun 12, 1905

By G. G. Barbante

Anode slimes produced during copper electrorefining are a valuable source of silver, gold, selenium and tellurium. The conventional pyrometallurgical process for treating slimes involves preliminary leaching in sulphuric acid followed by smelting in a reverberatory furnace with fluxes, but it is slow and has many recycle streams. The chemistry of the phases and the reactions that occur in slimes smelting are poorly understood and and this prevents major improvements to the process. Laboratory-scale experiments were conducted using unleached slimes, with and without the addition of fluxes and under neutral, oxidising and reducing conditions. Results show that selenium is readily removed as gaseous selenium dioxide and that molten Cu-Ag-Se-O phases form when fluxes are added. Oxidation-refining of these phases by air injection and flux addition can result in the formation of silver suitable for further electrorefining

Aug 1, 1995

By D. F. Malan

This study Investigates transient closure piles of tabular excavations. Measured closure profiles in stopes indicate that time-dependent acts f the rockmass can be very prominent but such effects have been largely neglected in past analyses and modelling. This was due to a poor understanding of the time-dependent mechanisms controlling closure rates This paper investigates the feas-ibility of representing the rockmass as a visco-elastic medium. Currently, no analytical solution for the viscoelastic convergence of a tabular stope is available in the literature. Therefore, the author derived a solution using the correspondence principle and a known elastic solution. It is assumed that the rockmass behaves elastically in hydrostatic compression and as a Kelvin substance in distortion A parametric study is Included to aid in the calibration of the model parameters, together with a discussion on the correct calibration of these parameters from experimental data.

Jan 1, 1995

By R. D. Leitch

"INTRODUCTION The character of mine drainage from areas of low pyritic coal3 and from average pyritic coal4 has been investigated, and to complete the study it seemed desirable to select a number of mines situated in high pyritic are as to determine whether or not this variation determines the relative acidity of drainage from mines operating in these characteristic coal fields. Advantage has been taken of some worked on in 1918 by Henry Leighton 5, then Professor of Economic Geology, University of Pittsburgh. He visited and has reported certain areas of high pyritic coal which we also visited during this study. Many of the mines were found to be idle in 1930 and a few were caved shut, apparently for several years. However, samples of the outflow from all mines visited were collected if possible and analyzed, and some general information was gathered for each mine. The map (fig. 1) shows the location of these areas as given by Leighton.ACKNOWLEDGMENTSThe information and assistance obtained from officials and others at the mines visited during this study are gratefully acknowledged, as well as the original suggestion from Dr. Glenn V. Brown of the State Sanitary Water Board who called attention to the desirability of such a study.Thanks are also especially due the coal laboratory of the United States Bureau of Mines, under the direction of H. M. Cooper, for the analyses and determination of sulphur forms in the large number of solid samples necessary to the work reported,This study has been carried on under the direction of R. R. Sayers, chief, health and safety branch, and W. P. Yant, supervising engineer, Pittsburgh Experiment Station, of the U. S. Bureau of Mines."

Jan 1, 1932

By Walter G. Steblez

The countries of Eastern Europe are former members of the Council for Mutual Economic Assistance (CMEA). Geographically, they are located in Central Europe (Poland, Hungary, Czechoslovakia) and Southeastern Europe, largely in the Balkans (Yugoslavia*, Bulgaria, Romania and Albania*). It is important to remember that all of the countries of Eastern Europe had central planning imposed on them by the Soviet Union during the years following World War II. "Stalinist" policy for industrial development had three important tenets: • central economic planning, or a nonmarket-based command economy with administratively set prices; • economic priorities that stressed the development of heavy industries such as mining, metallurgy (steel) and heavy machine building; and • self-sufficiency at all costs, which was aimed at abolishing reliance on the world capitalist market, or reducing it to a minimum. Essentially, the system of industrialization that was used in the Soviet Union in the 1930s and 1940s was imposed on Eastern Europe. Organic market economic development in Eastern Europe ceased during this period. The flaws of this experiment became apparent when mineral processing facilities were set up in many areas of Eastern Europe that did not have reliable resources. Poland, Hungary and Romania are good examples of this situation. The Soviet Union became the principal supplier of iron ore and other minerals and mineral fuels, not only to these countries but to the Bloc as a whole.

Jan 1, 1992

By C. S. Finney, John Mitchell

The introduction of ovens for the production of metallurgical coke is believed to be due to L. L. Norton who operated an iron foundry in the vicinity of Connellsville, Pa. Persuaded by his foreman, an English immigrant named Nickols from Durham, L. L. Norton put up a 12-ft square oven which produced coke in 1833. The coal used was taken from a local mine at Mounts Creek. The oven seems to have been used in conjunction with the customary method of coking in mounds. It was in the Connellsville district also, in 1841, that two carpenters, Provence McCormick and James Campbell, formed a partnership with John Taylor, a stone mason, for the manufacture and sale of oven coke. The task of the mason was to construct the ovens, while the carpenters were to build the arks by which the coke could be taken by water to the market at Cincinnati. The following account of the enterprise was given by McCormick: "James Campbell and myself heard in some way that I do not now recollect that the manufacturing of coke might be made a good business. Mr. John Taylor, a stone mason, who owned the farm on which the Fayette coke works now stand, and who was mining coal in a small way, was spoken to regarding our enterprise, and proposed a partnership-he to build the ovens and make the coke and Mr. Campbell and myself to build a boat and take the coke to Cincinnati, where we heard there was a good demand. This was in 1841. Mr. Taylor built two ovens. I think they were about 10 feet in diameter. My recollection is that the charge was 80 bushels. The ovens were built in the same style as those now used, but had no iron ring at the top to prevent the brick from falling in when filling the oven with coal, nor had we any iron frames at the mouth where the coke was drawn. The top and mouth had to be repaired when they fell in. In the spring of 1842 enough coke had been made to fill two boats 90 feet long-about 800 bushels each-and we took them to Cincinnati down the Youghiogheny, Monongahela, and Ohio, but when we got there we could not sell. Mr. Campbell, who went with the boats, lay at the landing some two or three weeks, retailing out one boatload and part of the other in small lots at about 8 cents a bushel. Miles Greenwood, a foundryman of that city, offered to take the balance if he would take a small patent flour mill at $125.00 hi pay, which Mr. Campbell did. He had it shipped here. We tried it, but it was no good, and we sold it to a man in the mountains for $30.00, and thus ended our coke business." So successful did the coke subsequently prove to be in use that the three partners were asked to deliver more. Evidently they had had enough of the coke business, however, for they refused to have anything more to do with it. Few ovens were built between 1841 and 1855, and it is reported that in the latter year, "there were only 26 coke ovens along the river above Pittsburgh". Successful coke makers of these years included Mordecai Cochran, Richard Brookius, and Colonel A. M. Hill. It was the use of coke in 1859 in the Clinton furnace erected by Graff, Bennett and Co. in a plant on West Carson Street, Pittsburgh, that brought the real beginning of the coke-iron era in America. Here the successful use of Connellsville coke as a blast-furnace fuel was demonstrated beyond all possible doubt, and from the year 1859 the coking industry expanded tremendously. The era of beehive coke ovens During the latter half of the nineteenth century and the early years of the twentieth, the major percentage of metallurgical coke produced in the United States came from beehive ovens. It was not until 1893 that the first battery of by-product ovens came

Jan 1, 1961

By E. T. Turkdogan

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

Jan 1, 1969