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By Arthur Taggart

A GENERAL awakening of interest among mill men concerning the mechanical efficiencies of their crushing machines is evident from a perusal of the recent files of mining publications. Considering the large part of the power bill which must be debited to the crushing department, such. interest is natural. When, however, the articles on the subject are read, the only statement upon which the writers agree is that fine grinding consumes a large amount of power, and that the machine which, from a concentration standpoint, offends as a slime producer is, for that reason, a serious offender in wasting power. When the mill man attempts to find a method for measuring the power wasted, or to compare the efficiency of one machine with that of another for the same work, he is confronted with a choice of methods which lead to conflicting results. There are two reasons why the work of crushing is not more generally understood. In the first place, experimental data are difficult to obtain; and in the second place, before these data can be put in general form certain assumptions must be made. A difference in these assumptions by different investigators has led to conflicting conclusions. This conflict has resulted in the proposal of two laws. The first of these is the so-called Rittinger's law, which is variously stated as follows: . "The work of crushing is proportional to the reduction in diameter."-R. H. Richards: Ore Dressing, p. 304 (1903). "The Work required to crush rock is very nearly proportional to the reciprocals of .the diameters crushed to."-A. Del Mar: Engineering and Mining Journal, vol. xciv, No. 24, p. 1129 (Dec. 14, 1912). "The Work done in crushing is proportional to the surface exposed by the operation, or better expressed for this purpose, the Work done on a given mass of rock is proportional to the reciprocal of the diameter of the final product, assuming that all the mass has been reduced to one exact size, which is only theoretically possible."- A. 0. Gates: Engineering and Mining Journal, vol. xcv, No. 21, p. 1039 (May 24, 1913).

Jan 1, 1914

Organisation Place Date 1918 American Society of Mechanical Engineers New York, N. Y. Dec. 3-6 Society for Promotion of Engineering Education, with British Educational Mission Cambridge, Mass. Dec. 6-7 Geological Society of America Boston, Mass. Dec. 28-31 American Association for the Advancement of Science Boston, Mass. Dec. 27- Jan. 2.

Jan 12, 1918

By Fred Bond

THE process of comminution by grinding is properly classified as an art, rather than as a science. Like most other operations concerned in ore dressing, or in the treat-ment of nonmetallic minerals, the mathe-matical relationships of rock breaking are still obscure, and much disputed. If some basic formula exists, comparable for in-stance to E = RI in electricity, it has not yet been placed in common use. The absence of such a comprehensive mathe-matical background undoubtedly is the cause of many inefficient designs and installations, as well as of much poorly oriented experimental work. On the other hand, the mathematical immaturity of the process constitutes an opportunity for a real contribution on the part of those who enjoy mental pioneering. Some of the statements made in any such exploratory work may be little more than opinions, and it is to be expected that some will later be proved untrue; but such an evolutionary development is necessary if we are ever to arrive at the fundamental laws, the discovery of which can change the empirical art into a mathematically exact science. The most significant principle of com-minution that we possess is probably Rittinger's law, which states that the work done in crushing or grinding is proportional to the area of the new surface produced. There is an alternative theory, known as Kick's law, which formerly was preferred to Rittinger's but which now is rather dis-credited. According to Kick, the work done in comminution is proportional to the volume, or weight, of the pieces broken, or to the cube of their diameters, while accord-ing to Rittinger it is proportional to the square of the diameters.

Jan 1, 1940

By Frank W. Osterwald

Violent, spontaneous destruction of coal faces and ribs during, what are commonly called, bumps endangers and at times destroys life and property in mines of the Book Cliffs coalfield, Carbon County, Utah. Because these mines supply much of the coking coal for the West Coast steel industries, mining is necessary, although costs are high and operating conditions are very difficult at times. As operations continue, mining will go to greater depths, and the difficulties will increase. Whether or not mining can be continued successfully depends in part on whether or not incidence of bumps can be controlled successfully. For this reason, the U.S. Geological Survey, at the request of and in cooperation with the U.S. Bureau of Mines, undertook a study of the Sunnyside No. 1 mine to determine what geologic factors were related to the incidence of bumps. This report presents the preliminary results of that study and indicates that some observable geologic features in the mine may be related directly or indirectly to bumps, and that other features may be used to infer stress distribution around workings that will aid in design of roof support measures. Coal is mined in the Sunnyside No. 1 mine from depths as great as 2500 ft by room-and-pillar methods. The surface topography is rugged with many steep cliffs and deep canyons, hence the load on the coal varies greatly within short distances. Much of the Sunnyside coal is under high stress, and while being mined, it shatters continuously' and falls from the face. Continuous shattering (bumping) makes mining easy, but if the shattering is interrupted, greater stress is built up and violent bumps may result when the coal is mined.

Jan 4, 1962

By R. G. Knickerbocker

THE copper smelter and refinery of The Messina (Transvaal) Development Co. Ltd., at Messina, South Africa, was erected in 1920 and 1921, but initial operations were deferred until late in 1922 on account of the collapse of the copper market in the interim. Because the anticipated production was to be only 20 tons of copper per day from a high-grade matte containing 60 per cent copper, and because the ore did not contain gold or silver in quantities sufficient to pay for separation from the copper bullion, it was decided to design the plant along lines quite different from the modern smelteries treating large quantities of sulfide ores carrying appreciable amounts of gold and silver. The plant was built, therefore, for the production of copper by the Nicholls-James process. By this method two-thirds of the copper matte produced was roasted in a Merton calciner and charged into a bath of the remaining one-third portion of unroasted matte in a reaction furnace. The original design was not only novel in providing for the Nicholls-James process, but also in comparison with new plants built elsewhere, because of factors inherent in the locality. Sources of supply for machinery were very remote; it takes three months after the placing of an order to accomplish delivery of machinery into Messina from the United States. Native labor was available at 30 to 40¢ per 8-hr. shift. These factors permitted plant design which provided no overhead cranes, no matte ladles, no slag pots or other usual mechanical means of transportation between departments. The design resulted in a compact simple plant with furnaces arranged close together and. terraced so as to provide for gravity transfer of molten material from one furnace to another and for manual disposal of products. Fig. 1 shows the relative location of furnaces. The three furnaces are parallel on successively decreasing elevations. A superimposed feed floor was provided above the furnaces. All three furnaces were provided with coal-dust burners served from a Bonnot system of coal-dust transportation, and the waste gases were discharged into waste-heat boilers.

Jan 1, 1932

By F. E. Jaumot, R. L. Smith

Self-diffusion in zinc has been used as an instrument for comparison of the absorption and sectioning techniques as a means of studying diffusion. Single crystal as well as poly-crystal samples were used asanda the temperature range of diffusion extended from 200° to 415°C. For temperatures above 200°C, the data indicate that the results obtained from the absorption technique agree with those obtained from the sectioning technique. The effect on the values of the diffusion coefficient of electroplating vs evaporation as a means of applying the tracer was investigated and no significant difference observed. It was found that an excess or deficiency of tracer did not materially affect the results obtained from the sectioning technique, but invariably caused errors with the absorption technique. NEARLY all self-diffusion experiments and many alloy diffusion experiments have employed radioisotopes as the instrument for following the diffusion. Of the various techniques in which radioisotopes are applicable, the two most widely used are the sectioning and absorption techniques. In the former, the diffusion coefficient is obtained from a curve of log concentration vs the square of the mean penetration depth. In the latter, the diffusion coefficient is calculated from a knowledge of the decrease in activity at the surface after diffusion. In spite of the importance of knowing the reliability of the diffusion data and the widespread use of these two techniques, they had not been directly compared experimentally on the same samples. Thus, such a comparison was worthwhile. The specific system chosen for this comparison was the self-diffusion of zinc, since the metal was readily obtainable in high purity, single crystals were easily grown, and the anisotropic features of the diffusion added an additional factor of interest to the comparison. Self-diffusion in both single and polycrystals was investigated, since the possibility existed that grain boundaries and grain boundary diffusion might produce different effects for the different techniques. Also, the effects of electroplating vs evaporation as a means of applying the radioactive tracer, and the effects of applying an excess or deficiency of tracer material were studied. The general experimental procedures and the mathematical analyses of both techniques have been described previously in some detail, and only those points essential to an understanding of the present work will be discussed here. The mathematical analysis of the sectioning data requires only a knowledge of the solution of Fick's equation. where C,, is the initial concentration, C is the concentration at depth x, D is the diffusion coefficient, and p is the absorption coefficient of the solvent metal for the radiation from the solute. Having obtained F from the experiment, the value of z can be read from a plot of F vs In z, and D can then be calculated if is known. The necessity of knowing the absorption coefficient causes most of the criticism of the absorption technique. It is very difficult to measure accurately under the conditions existing in the diffusion experiment, but it is absolutely necessary, as will be indicated briefly later. Portions of this problem have been discussed in detail elsewhere." The difficulties involved in the measurement of the absorption coefficient arise from three principle factors: the physical characteristics of the absorber, the geometry, and complex radiation spectra. The first two are heavily dependent upon the third. If

Jan 1, 1957

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page 1 Wilkes-Barre, Pa May, ?71 1 3 2 Bethlehem, Pa August, ?71 1 10 3 Troy, N Y November, ?71 1 13 4 Philadelphia, Pa February, ?72 1 17 5 New York, N Y May, ?72 1 20 6 Pittsburg, Pa October, ?72 1 25 7 Boston, Mass February, ?73 1 28 8 Philadelphia, Pa May, ?73 2 3 9 Easton, Pa October, ?73 2 7 10 New York, N Y February, ?74 211 11 St Louis, Mo May, ?74 3 3 12 Hazleton, Pa October, ?74 3 8 13 New Haven, Conn February, ?75 3 15 14 Dover, N J May, ?75 4 3 15 Cleveland, 0 October, ?75 4 9 16 Washington, D C February, ?76 4 18 17 Philadelphia, Pat June, ?76, 5 3 18 Philadelphia, Pa October, ?76 5 9 19 New York, N Y February, ?77 5 27 20 Wilkes-Barre, Pa May, ?77 6 3 21 Amenia, N Y October, ?77 6 10 22 Philadelphia, Pa. May, ?78 6 18

Jan 1, 1923

By Albert Sauveur

This paper explains the possibility of using advantageously a boiling solution of sodium picrate to reveal dendritic segregation in steel. The mechanism of the action of the reagent is described. The failure of manganese alone to produce persistent dendritic segregation is also considered. IRON, like other metals, solidifies through the formation of dendritic crystals; iron alloys forming solid solutions, like other solid solutions, solidify likewise through the formation of dendritic crystals. The alloying elements or impurities as well as the inclusions segregate generally in the interstices, or "fillings," between the axes and branches of the dendrites; that is, in the portions last to solidify. This results in dendritic segregation or heterogeneity, which is generally persistent and makes possible the revelation of the dendritic crystallization of the metal through the selective action of a suitable etching reagent.1 For this purpose, a cupric solution, such as Le Chatelier's, is generally used, copper being deposited on the pure, or relatively pure, ferrite present in the axes while the fillings remain free, or relatively free., from copper deposition. The dendritic structure, formed on solidification in a steel containing 0.50 per cent. carbon, 0.37 per cent. manganese, 0.12 per cent. silicon, 0.07 per cent. sulfur, and 0.035 per cent. phosphorus is shown, after treatment with Le Chatelier reagent, in Fig. 1 under a magnification of 8 diameters. Commercial steel always contains inclusions of manganese sulfide, which are located in the fillings of the dendrites. Comstock has shown that boiling sodium picrate imparts a dark coloration to these inclusions. We find that this reagent likewise reveals dendritic segregations in commercial steel, as shown in Fig. 2, under a magnification of 8 diameters, which represents the same spot as that shown in Fig. 1. The fillings

Jan 2, 1924

By Paul Tyler

THE ferroalloying elements are connecting links between the steel industry and the nonferrous metal industries. Although ferroalloys are distinctly nonferrous themselves, they serve the steel industry either in the manufacturing process or in modifying the product-in some cases so that it may compete in the markets with nonferrous metals. Of the 92 elements generally accepted by chemists as constituting the primary building blocks of matter, all but the very rarest have been investigated with a view to employing them in steel manufacture. The surprising thing is that so few have been found commercially acceptable. Despite the relatively small number of elements involved, the employ-ment of alloys in steelmaking is one of the most complicated and probably one of the least well understood of modern industrial enterprises. A great deal has been written regarding the action of individual elements and a profuse and somewhat acrimonious literature covers pretty much the whole field of ferroalloy ore supplies. In the middle ground between the miner and the steelmaker developments are less carefully watched by most observers, and except for an occasional description of the technique of some conversion process or the tariff hearings in Congress, very little is said about them. The purpose of the present paper is to describe in relatively nontechnical terms this highly complex industry and to study its relations to our national progress.

Jan 1, 1933

By Lennart Bergstedt, Olov Fägremo

Boliden Metall Aktiebolag, the prime base metal mining company of Sweden, treats some 10-10.9 t/y (11-12 stpy) of sulphide ore in nine concentrators. During the years considerable effort has been devoted to the development of all phases of the technology of ore prospecting, mining, milling, smelting and refining. This has been necessary due to the complex and low grade ores. The autogenous grinding technique was first studied within the company as early as 1945. Basic test work commenced during the early fifties, whereby the merits of pebble grinding could be evaluated. In parallel with the converting of the rod mill/ball mill grinding systems to rod mill/pebble mill systems, the development work concerning the feasibility of autogenous grinding went on resulting in the installation of a 8 6.7 x 2.1 m (8 22 x 7 ft.) cascade mill at the Vassbo lead mine in 1959. Long term tests at the Vassbo plant together with a number of pilot plant test involving low grade silicious ores and pyritic comples base metal ores successive led to a better understanding of the process of autogenous grinding. Before a two stage autogenous grinding system could be chosen for the expansion of the Aitik copper mine, a carefully planned survey concerning grinding characteristics and variances in the ore and flowsheet was undertaken. The expanded plant went on stream in 1972 and in the beginning of 1973 and since then has performed excellently.

Jan 1, 1979

By Morris Cohen

IT has been known for several years that in certain age-hardenable alloys precipitation of finely divided particles occurs simultaneously with the changes in physical properties; while, in other alloys, these changes take place prior to, or without any, precipitation. . The silver-copper alloys are generally considered to be the classical example of the first group, and the aluminum-copper alloys (duralumin) are typical of the second group. The two types of aging are explained by the precipitation theory and the knot theory respectively. ? It is well recognized now that these theories do not conflict with each other; the one used for a given aging system depends upon which way the alloy in question happens to age-harden. However, previous work on the aluminum-copper alloys1,2 has shown that if the aging temperature is raised sufficiently the hardening will be accompanied by actual precipitation. In fact, it is quite probable that all of the so-called knot-hardening alloys will harden by precipitation at elevated temperatures. Therefore, a combination of the knot and precip-itation theories is necessary to give a complete picture of the age-harden-ing of these alloys, and indicates that knot formation and precipitation are not independent processes. To test the generality of this concept, it is necessary to show that the alloys that commonly harden by precipitation will harden prior to precip¬itation if the aging temperature is sufficiently lowered. For this reason, it would be well to carefully re-examine the aging characteristics of the silver-copper alloys at aging temperatures somewhat below those used by previous investigators. If hardening can be detected prior to precipi¬tation in these alloys, it will lend great weight to the idea that knot forma-

Jan 1, 1936

By G. V. Woody, J. D. Price

Many producers of by-product coke have spent considerable time and given considerable thought to the use of a substitute for low-volatile coal as an admixture with high-volatile coking coal for charging high-temperature by-product coke ovens. Generally speaking, there are two principal reasons for this, one being occasioned by the lack, in certain localities, of low-volatile coal delivered at a cost sufficiently low to permit its use, and another being the desirability of finding a substitute product with a delivered cost lower than the cost of the low-volatile coal. It was for the first of these reasons that the Colorado Fuel and Iron Corporation was particularly interested in this subject. This paper deals with the experimental work and the results obtained by that company in producing and using low-temperature char. Overcoming Defects in Coke from Colorado Coals Colorado coking coals are all of the high-volatile type and were all laid down during the Cretaceous period, which makes them something like 80 million or so years younger, geologically, than eastern coals. They behave, when coked alone, something like the Pittsburgh-seam coals. They make a very brittle, highly cross-fractured, fingery coke of fair shatter value but quite low in resistance to abrasion. Mixed with a low-volatile coking coal such as Poca- hontas or certain Oklahoma coals, they make a coke that is equal to virtually any of the eastern cokes. The inferior quality of Colorado coke has long been recognized, and a considerable amount of time, effort and money has been spent upon investigations of means for improving its physical properties. While it has been found that some improvement in quality of coke can be secured by the adjustment and control of such variables as pulverization, moisture content, oven temperature and bulk density of charge, and through the addition of certain inert materials such as pulverized coke breeze, pitch, high-volatile noncoking or semicoking coal, the benefits so gained have been comparatively small. There are no low or medium-volatile coking coals available within a reasonable freight-cost distance. Therefore a substitute for low-vol-atile coal was developed through low-tem-perature carbonization—or, more correctly speaking, through the partial devolatiliza-tion—of high-volatile coals. The blending of this lower volatile char with the high-volatile coking coal distinctly improves the quality of coke made from Colorado coal. There is nothing especially new about this idea. In 1908 a Japanese patent was taken out by Kotaro Shimomura, whose claim was: The method of making a nonfingery coke out of bituminous coals, without using natural coals of low-volatile matter; according to which a certain coal is heated at a temperature between about 300°C. and about 600°C. so as to leave about 15 to 25 per cent volatile matter in the coal; this coal is mixed with the

Jan 1, 1944

By J. D. Price, G. V. Woody

Many producers of by-product coke have spent considerable time and given considerable thought to the use of a substitute for low-volatile coal as an admixture with high-volatile coking coal for charging high-temperature by-product coke ovens. Generally speaking, there are two principal reasons for this, one being occasioned by the lack, in certain localities, of low-volatile coal delivered at a cost sufficiently low to permit its use, and another being the desirability of finding a substitute product with a delivered cost lower than the cost of the low-volatile coal. It was for the first of these reasons that the Colorado Fuel and Iron Corporation was particularly interested in this subject. This paper deals with the experimental work and the results obtained by that company in producing and using low-temperature char. Overcoming Defects in Coke from Colorado Coals Colorado coking coals are all of the high-volatile type and were all laid down during the Cretaceous period, which makes them something like 80 million or so years younger, geologically, than eastern coals. They behave, when coked alone, something like the Pittsburgh-seam coals. They make a very brittle, highly cross-fractured, fingery coke of fair shatter value but quite low in resistance to abrasion. Mixed with a low-volatile coking coal such as Poca- hontas or certain Oklahoma coals, they make a coke that is equal to virtually any of the eastern cokes. The inferior quality of Colorado coke has long been recognized, and a considerable amount of time, effort and money has been spent upon investigations of means for improving its physical properties. While it has been found that some improvement in quality of coke can be secured by the adjustment and control of such variables as pulverization, moisture content, oven temperature and bulk density of charge, and through the addition of certain inert materials such as pulverized coke breeze, pitch, high-volatile noncoking or semicoking coal, the benefits so gained have been comparatively small. There are no low or medium-volatile coking coals available within a reasonable freight-cost distance. Therefore a substitute for low-vol-atile coal was developed through low-tem-perature carbonization—or, more correctly speaking, through the partial devolatiliza-tion—of high-volatile coals. The blending of this lower volatile char with the high-volatile coking coal distinctly improves the quality of coke made from Colorado coal. There is nothing especially new about this idea. In 1908 a Japanese patent was taken out by Kotaro Shimomura, whose claim was: The method of making a nonfingery coke out of bituminous coals, without using natural coals of low-volatile matter; according to which a certain coal is heated at a temperature between about 300°C. and about 600°C. so as to leave about 15 to 25 per cent volatile matter in the coal; this coal is mixed with the

Jan 1, 1944

By Myrick N. Bolles

The concentration of gold and silver in mattes low in copper, and the subsequent separation and recovery of either or both of these metals, is a question the satisfactory solution of which has long vexed metallurgists. It covers a broad and important department of metallurgical science and brings in its train a series of attendant problems continuing from the initial operations of concentration to the final recovery of " values."

Jan 1, 1905

By E. Just

The mining industry is guaranteed an important future because its products are indispensable. However, this can be anything from a brilliant, efficient, profitable future to one of being a heavy-handed, dull-witted claimant for public handouts, according to the caliber and training of the young men who enter the industry. Many views have been expressed about the type of education needed for today's mining industry. Criticisms have been aired to the point that further controversy amongst ourselves could be detrimental to both mining education and the mining industry. It is time we get together and start going somewhere. To canvass the various attitudes of mining educators, a questionnaire was sent to a group of these dedicated, intelligent men, whose primary interest is to help the industry and the profession. The following is a summary of their views.

Jan 9, 1961

By James Douglas

The Copper Queen mine was opened in 1880 by Messrs. Martin, Ballard & Reilly, and the first copper-furnace was blown-in on August 20th of that year. Prior to that summer nothing but prospect-work had been done on the copper Queen and on a number of adjacent claims. In fact, it was a small deposit, not of copper-ore, but of cerussite, which still remains undeveloped, on the western slope of the Queen hill, which

Jan 1, 1900

By G. W. Brock

Experiments in the form of aging of overstrained tension specimens and elevated temperature tension testing, have been carried out on recrystallized arc-cast molybdenum. The aging behavior of molybdenum was found to be strongly dependent on the degree of plastic strain present in the lattice: the reason for this being the low solid solubility for the common interstitial elements in molybdenum. GEORGE W. BROCK, formerly Research Associate, Department of Theoretical and Applied Mechanics, University of Illinois, Urbana, III., is Research Associate, Department of Engineering Sciences, IBM Research Center, Yorktown Heights, N. Y. Manuscript submitted January 19, 1961. IMD THE term strain aging is familiar in connection with the recovery of the yield point in mild steel after tensile overstraining, and there are other instances where it is known to exert an appreciable effect on mechanical properties. For example, steel exhibits a greater tensile strength at mildly elevated temperatures than at room temperature and serrated stress-strain flow curves occur under certain conditions. It has been known for a number of years that the phenomenon of strain aging is directly connected with the presence of carbon and nitrogen in the lattice; and extremely small amounts of either element are sufficient to produce the effect. In this study, the aging behavior of overstrained tensile specimens of recrystallized molybdenum has

Jan 1, 1962

By N. H. Emmons

THE work of a consulting engineer or manager, when controlling mining-operations, requires that he have all the information concerning the mine in as concise a form as possible, and as the ore-reserves and their depletion and enlargement are the vital points to be studied, it is well to have them kept up to date and in some convenient form. The present paper describes a method adopted by me, which shows in a very clear manner the ore-reserves in a mine. The case illustrated is that of a vein near enough to the vertical for the vertical elevation of the mine to be the main working-map. A flat ore-body would be represented on a similar plat, but instead of the horizontal thickness of the vein being shown in the circles, the vertical thickness would be inserted. Fig. 1 represents an ideal longitudinal elevation of a mine, plotted in the ordinary way, using 100-ft. blocks and section-lines. In a mine where the block-numbers are posted by the engineer underground, the system of keeping the ore-tonnages extracted from the different blocks is easily maintained, and the actual tonnages of ore extracted can be kept so that the surveyor can have a check on his estimate from time to time. The ore-reserve sheet, Fig. 2, should be the same size as the map it is to accompany. Each square is used for the description of the ore-reserve in the block it corresponds to on the elevation. Where the section-lines cross the levels a circle is drawn, in which are written the widths of ore at that point, these widths being used in the calculations of each block cornering in the circle. It has been found convenient to show the figures in black in the lower half of the circle when the actual widths of ore are known, and when it is necessary to make up the figures of probable ore, as at the time of making

Jun 1, 1912

By E. T. Turkdogan, Klaus Schwerdtfeger, P. Grieveson

The rate of growth of "Fe4N" on a iron was measured by nitriding purified iron strips in flowing am -monia -hydrogen gas mixtures at 504" and 554°C. It is shown that a dense nitride layer is formed when a zone -refined iron is used in the experiments. With less pure iron, the nitride layer is found to be porous. Through theoretical treatment, the self-diffusivity of nitrogen is evaluated porn the parabolic rate constant, and found to be essentially independent of nitrogen actirlity, e.g., D* = 3.2 x l0-12 and 7.9x l0-12 sq cm per sec at 504" and 554?C. Some consideration is given to the mechanism of diffusion in the nitride phase. THERE is a great deal of background knowledge on the solubility and diffusivity of nitrogen in iron, and on the thermodynamics and crystallography of several phases in the Fe-N system. Although case-nitrided steels have many applications in practice, no work seems to have been done on the diffusivity of nitrogen in the iron nitride, ?', phase. The only work reported on the related subject of which the authors are aware is an investigation by Prenosil,1 who measured the growth rate of the e phase on iron by nitriding in ammonia-hydrogen gas mixtures. EXPERIMENTS Purified iron plates of approximate dimensions 1 by 0.5 by 0.03 cm were nitrided in flowing mixtures of ammonia and hydrogen, in a vertical furnace fitted with a gas-tight recrystallized alumina tube. After a specified time of reaction, the sample was cooled to room temperature by withdrawal to the water cooled top of the reaction tube. The furnace temperature was controlled electronically in the usual manner within *l°C; the temperature was measured using a calibrated Pt/Pt-10 pct Rh thermocouple. For each experiment the iron strip sample was cleaned with fine emery cloth and degreased with tri-chloroethylene prior to the experiment. The ammonia-hydrogen gas mixtures were prepared from anhydrous ammonia and purified hydrogen using constant pressure-head capillary flowmeters. The gas mixture flowed upward in the furnace with flow rate of 400 cc per min at stp. The composition of the gas mixture was checked by chemical analysis at regular intervals. In most cases, the compositions of the exit gas and metered input gas agreed within about 0.3 pct, indicating that cracking of ammonia did not pose a problem at the temperatures employed. Two series of experiments were carried out using two different types of purified iron samples. In the first series of experiments at 550°C, vacuum carbon deoxidized "Plastiron" was used. The main impurities present in this iron were, in ppm: 4043, 50-Cr, 20-Zr, 40-Mn, 20-P, 20-S, 20-C, 50-0, and 10-N. In these experiments the rate data were obtained by measuring the change in weight of the iron specimen suspended in the hot zone of the furnace by a platinum wire from a silica spring balance. The nitride layer formed in these experiments was found to be porous, particularly near the outer surface. In other experiments, high purity zone-refined iron (prepared in this laboratory) was used. The total impurity content of this iron was 30 ppm of which 20 ppm was Co + Ni, 4 ppm 0, other metallic impurities were less than 1 ppm. The zone-refined iron bar, -2.5 cm diam, was cold rolled to a thickness of about 0.03 cm and the specimens were prepared for the experiment as described earlier. After the nitriding experiment, the sample was copper plated electro-lytically and mounted in plastic for metallographic polishing. After polishing, the thickness of the ?' layer was measured using a metallographic microscope. The nitride layer formed on the zone-refined iron was essentially free of pores. RESULTS The different morphology of the nitride layers grown on "Plastiron" and zone-refined iron is shown in Fig. 1. Both samples were nitrided side by side for 55 hr. The holes in the less pure iron, Fig. l(a), are confined to a region about one half thickness from the outer surface. The dense layer grown on zone-refined iron, Fig. l(b), is thinner than the porous layer on the "Plastiron". The impurities in the iron are believed to be responsible for the formation of a porous nitride layer. The pore formation may be due to the high nitrogen pressures existing within the nitride layer, e.g., the equilibrium nitrogen pressure is 1.2 x l05 atm in the 38.6 pct NH3-61.4 pct H2 and 6.6 x l03 atm at the Fe-Fe4N interface at 554°C and 0.96 atm. It is possible that the oxide inclusions present in the electrolytic iron may facilitate the nuclea-tion of nitrogen gas bubbles within the nitride layer. Support for this reasoning is the fact that pores are only encountered in the outer range of the layer where nitrogen pressures are largest. The photomicrographs in Fig. 2 show the effect of reaction time on the thickness of the dense nitride layer formed on zone-refined iron. These sections are from samples nitrided in a stream of 29 pct NH3-71 pct H2 mixture at 554°C for 22, 70, and 255 hr. In all the sections examined the nitride-iron interface was noted to be rugged. These irregularities are be-

Jan 1, 1970

By Nicholas J. Grant, John Chipman

A FULL understanding of the behavior of sulphur in the basic open-hearth process has been delayed by lack of dependable data covering a wide range of slag conditions in the absence of other complicating factors that are likely to be present under operating conditions. It has been generally accepted that strongly basic slags will dissolve more sulphur than will those in which the acidic and basic constituents are more nearly balanced. It has been known that both slag and metal would absorb sulphur from the flame when the sulphur content of the fuel is high. It has been generally believed that manganese assists in the transfer of sulphur from metal to slag. Almost nothing has been known of the effect of temperature upon desulphurization; the data have been conflicting and there has been a tendency to depend rather heavily upon analogy with the better understood desulphurizing reaction of the blast furnace. Many attempts have been made to build up from open-hearth data a satisfactory theory of the chemical reactions involved in the process. That this has been an extremely difficult task is owing to two reasons that have been very generally recognized. The first is the parallel and simultaneous reaction of sulphur transfer between flame and bath. The second is the difficulty of distinguishing between the factors that ultimately limit the transfer from metal to slag-i.e., equilibrium conditions-and those whose influence is only upon the rate of transfer. It has been the object of the work here recounted to study the equilibrium distribution of sulphur between slag and metal in the absence of these complicating factors, with the hope that a better understanding of the equilibria involved would lead to a better control of the over-all process in the open-hearth furnace. A review of the literature on steelmaking reveals almost complete agreement with respect to the paramount importance of lime in promoting desulphurization. In expressing this effect in quantitative terms, however, and in formulating the relationships between the concentrations of other slag components and the desulphurizing power, there is little agreement. For instance, the "basicity" or basic strength of the slag is commonly measured by some kind of ratio of concentration of basic to acidic oxides. Of these, the following have been reviewed by Schenck :20 [ ] Among others there appear the following:

Jan 1, 1946