Search Documents

By Shun-ichi Satoh

A NEW method of treating steel by ammonia has recently been intro¬duced into the metallurgical industry, by means of which piston cylinders of internal combustion engines, shafts and other similar steel products can be made more resistant to wear than formerly. In 1929 the writer' published the historical notes and some experiments upon nitrification. He believes that the corrosion of nitrified steel is a matter of importance and worth studying; and as there have been few studies thereof, he has conducted experiments in this respect. L. Guillet,2 in 1927, reported corrosion tests made on nitrified and cemented steels with acid and salt solutions. In 1928, 0. Hengstenberg3 reported the high resistance of nitrified steel to water vapor and air. V. 0. Homerberg4 stated that nitrified steel has high resistance to water, air and salt solution; and G. Hagg5 studied nitrified layers of iron by means of the X-ray. Though F. Hanaman6 in 1913, measured the single potential difference of steel treated with ammonia at above 650° C., no one, it seems, has ever measured the single potential difference of the so-called nitrified steels having extraordinary hardness. The writer measured the single potential differences of nitrified special steels in various solutions with the object of studying the corrosion problem and, if possible, of knowing whether any new physical property would be caused by nitrification.

Jan 1, 1932

By K. G. Kreider, J. H. Brophy, J. Wulff

The technology of nickel-activated sintering of tungsten powder has been successfully applied to the densification of plasma-sprayed tungsten. Nickel was added by infiltration in a zinc solution followed by evaporation of the solvent. After sintering one hour at 1300°C density 95 pct of theoretical and transverse rupture strength of 74,000 psi were obtained. Shrinkage was found to be anisotropic and the mechanism of densification was comparable to that found in the nickel-activated sintering of tungsten powder. 1 HE use of a plasma spray gun for the fabrication of massive tungsten parts has become increasingly interesting. Applications now exist where a deposit in the as-sprayed condition is satisfactory. However, these deposits are generally characterized by a lamellar anisotropic microstructure containing 15 pct porosity of which, typically, two-thirds is open to the surface. Mechanically, the as-sprayed deposits fail at relatively low stress levels with a biscuit-like fracture. As a result of these problems the possibility of improving structure and strength by sintering treatments subsequent to spraying is particularly attractive. Preferably this sintering treatment should be adaptable to large bodies of sprayed metal. The similarity between the as-sprayed tungsten structure and that of a powder compact suggests that the relatively low-temperature activated sintering technique1 might be profitably employed in the densification of plasma-sprayed tungsten. It was the purpose of the present investigation to develop a technique for introducing the nickel-activating agent into the sprayed structure, to evaluate the amount and mechanism of densification obtained as a function of time and temperature, and to obtain an indication of the relative strength before and after sintering. EXPERIMENTAL PROCEDURE Powder used for spraying was purchased from the Wah Chang Corp. in several size fractions ranging from an average size of 4 to 150 . These powders were sized further for an explicit study of the influence of average feed size on densification. All powders were dried at 200°C before use. Spraying was accomplished with a Plasma Flame unit manufactured by Thermal Dynamics Corp. Several modifications of the unit were helpful in conducting the investigation. A variable speed auger feed mechanism coupled with the carrier gas mecha nism facilitated the use of fine particle sizes. A coil of ten turns of copper tubing in series with the arc power and concentrically would around the nozzle improved nozzle life and extended the range of operating currents available. The function of the auxiliary coil was to cause the arc to spin and to prevent impingement at only one point in the nozzle. Normally air sprayed deposits were made with an arc maintained at 400 amp at 50 to 70 v. The arc was blown by a gas mixture containing from 5 pct H, 95 pct N for the finest powder feed sizes ranging to 20 pct H, 80 pct N for the coarsest size. The flow rate was maintained at 100 cu ft per hr NTP through a nozzle of 0.25 in. ID. When apraying in air, the powder stream was directed toward an aluminum substrate for ease of mechanical removal of the deposit. The substrate was cooled by diverting the plasma flame with an air jet, and a second jet was directed on the deposit surface. In this configuration a gun-to-work distance of 2 to 3 in. was found to be satisfactory. Fig. 1 represents a typical as-sprayed deposit micro-structure. Laboratory studies of protective atmosphere spraying were carried out in cylindrical chamber 8 in. in diam by 18 in. in length. In operating the nozzle attached to such a chamber, particular care was required to avoid nozzle burn out due to reduced gas flow. The structure and density of the chamber sprayed deposits varied over wide ranges depending on substrate temperature. For the purposes of this investigation, flat deposits were made approximately 2 in. sq by 3/8 in. thick. From these deposits individual samples were cut an ground to a rectangular shape typically 1 1/2 in. by 1/8 in. sq such that the long dimension was perpendicular to the spraying direction. For the study of shrinkage anisotropy deposits up to one inch thick were produced. From these, rectangular samples were cut having a longer dimension parallel to the spraying axis. Prior to the addition of activating agent, the samples were deoxidized in hydrogen at 800°C for 20 min. No detectable dimensional or microstructural change was observed after this treatment. The addition of nickel was accomplished by infil-

Jan 1, 1963

By A. M. Nicholas

WHEN attempting to lift mill pulp containing a considerable percentage of wolframite, in an ordinary bucket elevator, difficulty was encountered from the tendency of the tungsten minerals to settle, on account of their high specific gravity. Lifts not exceeding 20 ft. (6m.) could be accomplished without particular difficulty, because there was insufficient time for consolidation of the heavy minerals in the bottom of the bucket; but with higher lifts, the heavy tungsten minerals would settle so solidly that when the bucket turned over at the top of the elevator the contents could be only partially dumped. In this case it ,was necessary to lift the material a distance of 34 ft. (10m.); hence some means had to be adopted to prevent settling, at least to such an extent that the material could be dumped from the buckets. To reduce the carrying time to a sufficient extent would have required a belt speed of 475 ft. (144.7m.) per minute, which was not feasible. It was decided to try, by vibrating the belt about midway of its span, to keel) the material sufficiently agitated during elevation to prevent settling. Underneath the rising side of the belt was placed a 12-in. (30.48-cm.) idler pulley, 18 ft.-(5.5 in.) up in the total lift of 34 ft. The idler pulley was set eccentric by 3/4 in. (19 mm.) and it was hoped that the vibration thus imparted to the belt, running at a speed of 280 ft. (85 m.) per minute, would prevent settling in the buckets. It was found that the pressure of the belt on the idler, due to the small inclination of the elevator, was not sufficient to overcome sliding on the idler, and the agitation was insufficient to accomplish the desired purpose. The idler was then connected to the drive shaft of the elevator through an intermediate pulley, gearing down to a speed of 20 r.p.m., so that a positive vibration was imparted to the belt; this imparted enough motion to the belt to prevent settling and the contents of buckets clumped satisfactorily.

Jan 2, 1918

By Charles Fairhust

Although the term 'rock mechanics' started to become popular about the time of the First U.S. Rook Mechanics Symposium in 1956, study of the mechanical behavior of rock certainly pre-dates this event. Bucky, Phillips, Von Karman, Fayol, Galileo...the list of significant contributors can be traced back over centuries, - not surprising for the oldest structural material used by man. Started with a strong mining orientation by the Colorado School of Mines, University of Minnesota, and Pennsylvania State University, joined soon after by Missouri School of Mines and the University of Texas, the Annual U.S. Symposium on Bock Mechanics has evolved into the main U.S. form for discussion of all aspects of rock mechanics, basic and applied - tectonophysics to comminution; near-surf ace foundations to deep mine support design. Although dominantly a U.S. event the annual symposium has benefitted from regular and important contributions from abroad. It would be presumptuous to attempt a comprehensive statement of significant developments over the 25-year history of the U.S. Bock Mechanics Symposium. This anniversary address will attempt instead to present a personal view of developments that appear to be of broad general significance and that may indicate directions for the future. Among the developments to be discussed in the address arc the following: - Energy Basis of Book Fracture Early rock mechanics investigators often overlooked the important distinction between a failure initiation stress and structural collapse. Although essentially synonymous in the

Jan 1, 1984

By F. M. Drake

IN this paper I propose to describe a plant which I lately erected for the Mount Stewart Lead and Silver Mining Company of Leadville, New South Wales, Australia. I am indebted to Mr. W. F. Burrow, of the Roads and Bridges Department of New South Wales, for the drawings which I present herewith, he having reduced and assembled them from my working drawings. The works are situated on a sloping hillside, but sufficient fall mas not available to have the furnace as high as desired, and at the same time have a good slag-tip and sufficient depth on the ore-floor to store a supply of ore and flux. The ore is delivered on the ore-floor (which is of the full width of the furnace-building, and extends back into the hill a distance of seventy feet) by two overhead tramways (not shown in the drawings), one on each side. From these the ore-mixture is made up on one side, while it is being taken to the furnace from the other. The fuel also is delivered by these tramways. The fluxes are stored on a floor directly at the back of the boiler and engine room. The boiler is a Cornish one, 6 feet 6 inches in diameter by 25 feet long. Its flue is 3 feet in diameter and does not contain Galloway tubes. The working-pressure is 40 pounds per square inch. The engine is an old-fashioned one, with a cylinder 16 inches in diameter by 30 inches stroke. Both the engine and boiler had been part of the plant of a defunct gold-mining company. They were very extravagant in their consumption of fuel. The blast is supplied by a rotary pressure-blower, of the Baker pattern, made in England. It has a capacity of 60 cubic feet per revolution. The furnace, which has several novel points, is shown in detail in Figs. 1, 2 and 3. The jackets are of cast-iron, and are higher than those generally used. They are different, too, in that the feedwater inlet is through a hand-hole plate near the bottom. This plate is fastened to the jacket by stud-bolts, and is provided with a baffleplate, which prevents the cooling water from impinging against the inner plate. The outlet is by a goose-neck at the top, which dis-

Jan 1, 1893

By Sidney H. Haughton

WHEN the white pioneers of the eighteenth and nineteenth centuries advanced from the coastal settlements of southern Africa into the interior of the subcontinent, they found it inhabited, more or less sparsely, by brown or black peoples mainly of pastoral habits but equipped with a fighting spirit and certain fighting weapons. Some of the tribes were smiths, others were miners and metallurgists; all used fuel, either industrially or domestically. Some of that fuel was wood, some cattle dung, and in some places the natives mined outcrop coal. Coal was first discovered by Europeans in Natal about 1840. After proper deliberation and after allowing due time for a consideration of all the implications, the Natal Government decided in 1881 (40 years after) to import an English expert to investigate and report on the discovery. Things then moved rapidly, and in what to a geologist is the remarkably short space of eight years, Natal collieries were producing at the rate of nearly 30,000 long tons per annum or 100 long tons per working day!

Jan 1, 1945

By Robert Glass Cleland

THE BEGINNING of a large enterprise is often as in- significant as a lump of leaven hidden in a bowl of meal or a handful of mustard seed that the wind blows across a field. In 1950 the company known today as the Phelps Dodge Corporation had nearly thirty-two thousand stockholders, paid salaries and wages of about fifty million dollars to some thirteen thousand persons, produced nearly four hundred and ninety million pounds of copper, and possessed net current assets of approximately one hundred and six million dollars. For the origin of this great business, one must go back approximately a hundred and fifty years to an obscure saddle-making shop in the small town of Hart- ford, Connecticut. Anson Greene Phelps, proprietor of the shop and master saddler in his own right, was born in 1781-the year of the Battle of Yorktown, the surrender of Cornwallis, and the close of the Revolutionary War Anson's forebears had come to America in the great Puritan migration that left fields, shops, pulpits, and hearthstones in the reign of Charles the First to transplant the strong, tough roots of their race, culture, and institutions in the New World.

Jan 1, 1952

By Arthur Connolly

WHEN scientific literature was lacking or meager, research necessarily meant laboratory investigation above all else. Today, scientific literature has attained tremendous proportions, and the volume increases at a much faster rate than it is digested and efficiently utilized. For that reason the present-day research worker should spend much more time in the library, and correspondingly less in the laboratory, than is the general custom. Library research would overcome two serious errors often made by scientists: duplication of work described completely and failure to appreciate inventions described almost verbatim in the literature. To emphasize these failings that often occur in present-day research, consider a hypothetical scientist as he conducts his search from inception to the stage where it is made available to the public by patent or other publication.

Jan 1, 1942

By L. O. Howard

WHAT was perhaps the first attempt at basic converting in the Southwest was made by the late Charles F. Shelby at Cananea early in 1907, when he removed the acid lining from one of the 8 by 12-ft. barrel-type converters then in use at the reduction works of the Cananea Consolidated Copper Co. and substituted a lining of one course of magnesite brick. In this shell, he blew 21 taps (about 180 tons) of matte to white metal before the brick gave out along the tuyère line. In every case, the white metal so made was transferred and blown to copper in other converters. The cost of the lining was $700 and Mr. Shelby gave up the experiment as impracticable. No further serious effort to bessemerize copper mattes in a vessel having a more or less permanent lining of basic brick was made by any of the large copper smelters in the Southwest until some months after Messrs. Peirce and Smith had brought the question permanently before the public, and had proved it to be a metallurgical and financial success by their work at Baltimore and Garfield. Early in 1911, the Cananea Consolidated Copper Co. had in operation at its reduction works at Cananea, Mex., several 8 by 12-ft. barrel-type converters lined with magnesite brick which had previously been operating with acid linings. In the 18 months following, these converters produced 50,000 tons of copper. In June, 1912, this company installed the first of its new equipment of six stands of electrically operated 12-ft. Great Falls type converters, and shortly afterward discontinued the use of the smaller shells. In September, 1911, the Consolidated Kansas City Smelting & Refining Co. had installed at its El Paso plant two 10 by 26-ft. Peirce-Smith converters. Later, in March, 1913, one standard Great Falls type converter was added. .About the time the Peirce-Smith converters were going in at El Paso, the Calumet & Arizona Mining Co. was experimenting with basic linings in 7-ft. by 10-ft. 6-in. barrel converters at its plant in Douglas, Ariz. These efforts were sufficiently successful to enable the plant to handle the total output of copper in these small shells until the standard. Great Falls converters were substituted in June, 1914.

Jan 9, 1916

By Clarence Linville

FULTON1 says: "Speiss is an artificial arsenide of iron containing smaller amounts of other metals. In constitution it is similar to a matte except that arsenic replaces sulfur." For the purposes of this paper it will be necessary to broaden the definition, and I propose the following: Speiss is an artificial mixture of arsenides, of which arsenide of iron may be taken as a type, but iron may be replaced in part or wholly by other metals (such as copper, nickel, cobalt, lead and zinc) and the arsenic may be replaced in part or wholly by antimony. In addition to antimony and arsenic, speisses often contain sulfur. Speisses usually also contain both silver and gold. Table 1 illustrates the variations that may be encountered. TABLE 1.-Speiss Analyses

Jan 5, 1925

By George B. Clark, John W. Brown, Hemendra N. Kalia, Ronald R. Rollins

A new theory for three dimensional collapse of conical liners shows why the two dimensional theory may offer a good approximation. Shaped charge design parameters and rock target properties were investigated to determine their effects on penetration and breakage. Penetration in dolomite is somewhat similar to that in steel, but copper does not have markedly better penetration capabilities than brass. Several metals, liner thicknesses, cone angles and standoff ranges for each were investigated. Effective standoff is greater for aluminum than more dense metals. Optimum geometry appears to approximate that for metal targets. Resistance to penetrations was greatest for a red granite and dense siliceous rocks, and least for dolomite and porous sandstone. Hardness and compressive strength appear to be two important conventional proper- ties. The first order law does not apply to the rocks tested. Dolomite may be drilled with shaped charges, the holes sprung and round blasted successfully.

Jan 1, 1971

Safety Factor Characteristic Curves. Their Application to Mine Hoisting Ropes. (Paper by W. A. Boyer, Transactions AIME, 199, 989; Mining Engineering, October 1954. Discussion by B. E. Grant.) ............................................................................................................................. 1101 The Use of Wooden Rock Bolts in the Day Mines. (Paper by Rollin Farmin and Carville E. Sparks, Transactions AIME, 196, 922; Mining Engineering, September 1953. Discussion by Edward Thomas.) ................................................................................................................................. 1101 An Analysis of Mine Opening Failure by Means of Models. (Paper by Bernard York and John J. Reed, Transactions AIME, 196, 705; Mining Engineering, July 1953. Discussion by J. P. Zannaras.) ... 1102 B — Minerals Beneficiation Flotation and the Gibbs Adsorption Equation. (Paper by P. L. de Bruyn, J. Th. Overbeek, and R. Schuhmann, Jr., Transactions AIME, 199, 519; Mining Engineering, May 1954. Discussions by W. E. Ewers and Masayoshi Wada.)........................................................................................... 1103 Manganese Upgrading at Three Kids Mine, Nevada. (Paper by S. J. McCarroll, Transactions AIME, 199, 289; Mining Engineering, March 1954. Discussion by J. Bruce Clemmer, J. B. Rosenbaum, and C. H. Schack.)............................................................................................................. 1105 A Physical Explanation of the Empirical Laws of Comminution. (Paper by D. R. Walker and M. C. Shaw, Transactions AIME, 199, 313; Mining Engineering, March 1954. Discussions by Dimitri Kececioglu, George B. Clark, and Fred C. Bond.) ......................................................... 1106 F — Coal Underground Electrocarbonization of Coal and Related Hydrocarbons. (Paper by T. C. Cheasley, J. D. Forrester, and Erich Sarapuu, Transactions AIME, 199, 908; Mining Engineering, September 1954. Discussions by John G. Tripp and James L. Elder.)....................................................... 1108 Longwall Mining and Mechanization, with Special Reference to Nova Scotia. (Paper by Frank Doxey, Transactions AIME, 199, 701; Mining Engineering, July 1954. Discussion by Louis A. Turnbull.) ........................................................................................................................................ 1109 Cleaning Various Coals in a Drum-Type Dense-Medium Pilot Plant. (Paper by M. R. Geer, W. A. Olds, and H. F. Yancey, Transactions AIME, 196, 696; Mining Engineering, July 1953. Discussion by John Griff en.)................................................................................................................................. 1110 Frontiers in Heat Extraction from the Combustion Gases of Coal. (Paper by Elmer R. Kaiser, Transactions AIME, 199, 304; Mining Engineering, March 1954. Discussion by G. A. Vissac.) ............ 1112 Exploration of the Oaxaca Coal Fields in Southern Mexico. (Paper by Luis Toron and Salvador Cortes-Obregon, Transactions AIME, 199, 505; Mining Engineering, May 1954. Discussion by John D. Price.).................................................................................................................. 1113 H — Industrial Minerals Alkali Reactivity of Natural Aggregates in Western United States. (Paper by William Y. Holland and Roger H. Cook, Transactions AIME, 196, 991; Mining Engineering, October 1953. Discussions by Dexter H. Reynolds and W. L. Merritt.) ......................................................... 1114 Characteristics of Titaniferous Concentrates. (Paper by L. E. Lynd, H. Sigurdson, C. H. North, and W. W. Anderson, Transactions AIME, 199, 818; Mining Engineering, August 1954. Discussion by D. R. Grantham.)........................................................................................................................ 1116

Jan 1, 1955

By Otto W. Nuttli

The magnetic method of prospecting is well suited to determination of faulting in the basement rock. In addition to establishing the horizontal position of the fault, it often furnishes valuable information concerning the depth and amount of faulting. Consider a simple case of a vertical fault, represented in cross-section in Fig. 1. Let AA' represent the plane of observation (ordinarily the surface of the earth), and BB'B"B"' the upper surface of the basement. Assume that the sedimentary rocks are nonmagnetic, so that the magnetic susceptibility of the material above the basement is zero. Let k indicate the susceptibility of the basement rock, a- the density contrast between it and the neighboring sedimentary rocks, and t the amount of vertical displacement.

Jun 1, 1955

By R. W. Shoenberger, J. E. McNulty, B. R. Kuchta, William Spackman, A. A. Terchick, M. E. Hopkins, Norman Schapiro, R. J. Gray, A. F. Duzy, M. P. Corriveau

INTRODUCTION * The United States is fortunate in having abundant reserves of metallurgical-grade coals. Although these coals are better in quality and more accessible than most metallurgical-grade coals found throughout the rest of the world, the best grades of these coals are being depleted. Consequently, more efficient exploration tools and techniques, such as advanced methods of core drilling and logging, correlation by petrography, paleontology, palynology, † physical stratigraphy, and geophysical methods are being used to help assess the extent and quality of the remaining coal reserves. Exploration and assessment of new and existing coal properties become of utmost importance in determining ( 1 ) the economic justification for mining the coal, (2) the optimum design of the preparation plant, and (3) the most effective use of the coal. Recent progress has been made in relating mineral matter, especially pyrite, in coal to geologic conditions and paleogeographic trends. l * Editor's note: Because of the numerous and varied contributions of the associate authors of this chapter, the text does not differentiate between sections prepared by each individual as has been done in other chapters. † Palynology is the science concerned with plant microfossils, especially spores. pollen. and other fossils of microscopic size.

Jan 1, 1979

The United States Coast and Geodetic Survey has announced the completion of a new outline map of the United States on the Lambert conformal conic projection, scale 1-5,000,000. This map is intended merely as a base to which may he added any kind of special information desired. The shore line is compiled from the most recent Coast and Geodetic Survey charts, state names and boundaries, principal rivers, capitals, and the largest cities in the different states are also embodied. The value of the new outline map on the Lambert projection can best be realized when it is stated that it shows that throughout the largest and most important part of the United States, that is, between latitudes 30 ½ and 49°, the maximum scale error is only 0.5 per cent. This amount of scale error of 0.5 per cent. is frequently less than the distortion due to the method of printing and to changes from the humidity of the air. Only in southernmost Florida and Texas does this projection attain its maximum error of 233 per cent. The map measures 25 inches by 39 inches and will be sold by the Government at 25 cents.

Jan 7, 1919

By Roshan B. Bhappu, Zeki M. Dogan

Two magnesite ores containing 3.15% and 8.73% SiO2 and a calcined magnesite product assaying 2.6% Si02 were first reduced in size to -20 mesh by roll crushing. 'They were then treated dry on a high intensity magnetic separator to reduce their silica content by rejecting iron-stained silicate minerals in the magnetic fraction and obtaining marketable magnesite or calcined magnesite as a nonmagnetic product.

Jan 1, 1975

By M. Streat, R. Y. Qassim

Summary This paper reviews the developments in uranium process technology as a result of modern trends in the design of ion exchange equipment. The operation of the Cloete-Streat fluidised bed contactor is described and pilot-plant development of this contactor for uranium slurry work at Imperial College is outlined. The properties of a suitable ion exchange resin for slurry treatment are discussed, together with a description of relevant rheological properties of ore suspensions. A prediction of ion exchange resin- slurry behaviour is presented in order to establish the feasible operating limits for this type of R-I-P contactor.

Jan 1, 1973

By S. K. Bose, P. K. Sahoo, S. C. Sircar, P. K. Jena

High grade manganese ores are utilized in metallurgical, chemical, and battery industries, whereas the low grade ores are not accepted for these purposes and hence get accumulated at the minehead. In the present study an attempt was made to solubilize the manganese value as its sulfate by roasting the low grade ore with a suitable sulfatizing agent followed by water leaching. The different parameters were determined in the laboratory scale. Based on these, kilogram scale experiments were conducted where an appreciable amount of manganese goes into solution during leaching.

Jan 1, 1981

By C. Law McCabe, R. G. Hudson

The Knudsen cell has been employed to determine the free energy of formation of Mn7Cs in the temperature range 800" to 950°C. A value of 66,440 cal was found for hH°o for a-manganese. Measurements of the pressure of manganese over a mixed carbide, (Fe,Mn),C, points to a power relationship between aun7cs and N.4,. RECENTLY Kuo and Perssonl have reported that the carbide of manganese which is in equilibrium with graphite at temperatures up to 1100° C is Mn7Ca. There are no published data on the thermo-dynamic properties of this compound. In order to determine the stability of Mn7Ca, it appeared that, by obtaining the pressure of manganese above 8-manganese and also above Mn,C, in equilibrium with graphite, the free energy of formation of Mn7Ca from 8-manganese and graphite could be obtained. In addition, the vapor pressure of manganese, reported by Kelley From data of Bauer and Brunner,' is subject to some uncertainty and further determinations of the vapor pressure of manganese seemed warranted. In this investigation of the pressure of manganese vapor above pure manganese and also above the carbide of manganese in equilibrium with graphite the apparatus used is the Knudsen orifice cell. The same apparatus, experimental procedure, and method of calculating the pressure was used in this investigation as in one previously reported.~ Care was taken to insure that the cells were at constant weight before using them in a run. The manganese charged in the cell was CP grade powder, carbon free, obtained from the Fisher Scientific Co. A spectroscopic analysis of the manganese after appreciable amounts of it had vaporized from the Knudsen cell showed that no element was present in sufficient quantities to contribute to a weighable weight loss or to decrease the vapor pressure of manganese to any appreciable extent. The spectro-graphic analysis was 0.002 pct Cu, 0.05 pct Fe, 0.002 pct Pb, and 0.002 pct Ni. 8-manganesea is the allo-tropic form of manganese which was present in the cell at temperatures used in this investigation. The manganese carbide, Mn,Ca, was made in the following way: In a closed graphite cell manganese powder was added to graphite powder, which was made from graphite rods for spectrographic use. The manganese powder was the same as that described previously; 5 pct excess graphite was added over that required for the formation of Mn7C,. The mixture was heated in a closed graphite cell for approximately 20 hr at 1350°K under vacuum. X-ray analysis revealed that there was no manganese present after this treatment, but that the lines due to Mn,C, were present. In order to prove that there was no volatile carbide of manganese which was effusing out of the cell, the following experiment was performed: A graphite effusion cell containing graphite power, in excess of that to form Mn,C, of a desired amount, was brought to constant weight on heating at 1228°K. The required amount of manganese was accurately weighed and then added to the graphite effusion cell. The cell was placed in a vacuum at 1228°K for one week, which was the time calculated for the manganese to have effused completely, assuming instantaneous formation of Mn,C8. The cell was then weighed again. This experiment was carried out on two different occasions and both times the weight loss of the cell came within 1 pct of the weight of manganese originally charged minus the weight of manganese left in the cell, as determined by chemical analysis. These data are summarized in Table I. This agreement is considered to be within experimental error and is taken as proof that no carbide of manganese is volatile in this temperature range. It was established, by X-ray analysis, that Mn,C, formed before appreciable amounts of manganese vaporized from the metal powder which was charged. The identification of the carbide of manganese which was present in the Knudsen cell in equilibrium with graphite and manganese vapor was carried out by Kehsin Kuo at the University of Uppsala. He established that the authors' sample, which was submitted to him for analysis, contained the phase

Jan 1, 1958

By S. Gilbert, G. R. Bailey

A further evaluation of the bomb-sampling method for determining the oxygen content of liquid steel is presented. The results of this study and their close agreement with the results of an earlier evaluation confirm the conclusion that the bomb-sampling method is valid for obtaining representative samples for the determination of the oxygen content of a liquid steel bath. WHAT constitutes the most desirable procedure for obtaining a sample suitable for determining the oxygen content of a liquid steel bath has been a controversial subject for several years. In 1952 Huff, Bailey, and Richards' described a modification of the bomb-sampling technique originated by McCutcheon and Rautio.' In both the modified and original techniques, a small cast-iron or steel mold containing aluminum wire and appropriately covered is inserted into the furnace, coated with slag, and then plunged into the metal bath. Upon entering the metal, the cover melts and a sample of the steel bath enters the mold. The data presented by Huff, Bailey, and Richards' indicated that reproducible samples could be obtained by their method. Furthermore, the oxygen analyses from samples obtained by their method agreed better with those from controlled laboratory experiments than did analyses from samples obtained by methods previously suggested for sampling large liquid-metal baths. Most techniques, other than bomb-sampling, require that a sample of liquid steel be removed from the furnace in a well slagged spoon and poured into an iron mold containing aluminum or into a massive copper mold for rapid chilling. Pouring in this manner requires that the sample pass through the air. The controversy, then, is somewhat as follows: Proponents of the spoon-sampling method and similar dip-and-pour methods feel that the introduction of a cold steel mold into a molten steel bath may result in a localized boiling condition that may deplete the steel of oxygen to a significant degree in the area where the bomb is introduced. Conceivably this boil could cause results that are, on the average, too low and nonrepresentative of the bath composition. On the other hand, samples that are spooned and then poured through the air may also be nonrepresentative because of oxidation by the atmosphere. The restrictions imposed in sampling with a spoon are much more stringent than those imposed when sampling with the bomb-type mold within the furnace. The spoon sample must be taken in a well slagged spoon, a requirement that depends on the condition of the slag in the furnace. Also, the samples must be poured as quickly as possible, without shaking the spoon and without allowing slag to enter the mold. The necessity of fulfill-

Jan 1, 1955