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By Robert C. Stephenson

Large deposits of titaniferous magnetite occur associated with anorthosite and gabbro in the Lake Sanford area, Essex County, New York. The ore, gabbro, and anortbosite show consanguineous relations. Anorthosite grades through gabbroic anortbosite into gabbro but is locally intruded by gabbro. Structural and petrographic evidence suggests that gabbro was differentiated from anorthosite by filter pressing. Field and laboratory study of ore occurrences indicates that an ore residuum concentrated in the gabbro through magmatic segregation' by normal crystallization and flowage. Ore occurs as bands which grade into gabbro, and also as large masses which replace anorthosite. Ore in the gabbro is finer grained and richer in ilmenite than ore in anorthosite. Introduction The Lake Sanford area lies in the heart of the Adirondack Mountains, in the southeast portion of the Santanoni Quadrangle (Fig. I), and there are four ore bodies in the area immediately surrounding Lake Sanford. The area lies 30 miles by highway from the railroad at North Creek. The deposits were discovered in 1826, and from then until 1858 iron was produced in small quantities. They were idle from 1858 to 1906. Between 1906 and 1913, extensive development work was carried on. These early attempts to produce iron ore were thwarted by transportation difficulties and by the titanium content of the ore, which, ironically, has been the element responsible for the present development. In 1941 the National Lead Co., Titanium Division, developed the Sanford Hill ore body and is now producing ilmenite and magnetite concentrates.18 The Defense Plant Corporation is extending the railroad to the property from North Creek and is building a sintering plant to treat the magnetite concentrate. Investigations OF the Deposits* Early studies of the Lake Sanford titaniferous magnetite deposits were made by Emmons in 1842,l2 by Kemp, in 1897-98'0 and by Newland in 1908.22 Singewald26 and Osborne23 considered these deposits along with numerous other titaniferous magnetite deposits in 1913 and 1928, respectively. None of these reports entailed a detailed study of the ore occurrence in this area. The present study was begun in 1940. Seven months were spent in the field, and considerable time was spent in labora-

Jan 1, 1949

By Robert C. Stephenson

Large deposits of titaniferous magnetite occur associated with anorthosite and gabbro in the Lake Sanford area, Essex County, New York. The ore, gabbro, and anortbosite show consanguineous relations. Anorthosite grades through gabbroic anortbosite into gabbro but is locally intruded by gabbro. Structural and petrographic evidence suggests that gabbro was differentiated from anorthosite by filter pressing. Field and laboratory study of ore occurrences indicates that an ore residuum concentrated in the gabbro through magmatic segregation' by normal crystallization and flowage. Ore occurs as bands which grade into gabbro, and also as large masses which replace anorthosite. Ore in the gabbro is finer grained and richer in ilmenite than ore in anorthosite. Introduction The Lake Sanford area lies in the heart of the Adirondack Mountains, in the southeast portion of the Santanoni Quadrangle (Fig. I), and there are four ore bodies in the area immediately surrounding Lake Sanford. The area lies 30 miles by highway from the railroad at North Creek. The deposits were discovered in 1826, and from then until 1858 iron was produced in small quantities. They were idle from 1858 to 1906. Between 1906 and 1913, extensive development work was carried on. These early attempts to produce iron ore were thwarted by transportation difficulties and by the titanium content of the ore, which, ironically, has been the element responsible for the present development. In 1941 the National Lead Co., Titanium Division, developed the Sanford Hill ore body and is now producing ilmenite and magnetite concentrates.18 The Defense Plant Corporation is extending the railroad to the property from North Creek and is building a sintering plant to treat the magnetite concentrate. Investigations OF the Deposits* Early studies of the Lake Sanford titaniferous magnetite deposits were made by Emmons in 1842,l2 by Kemp, in 1897-98'0 and by Newland in 1908.22 Singewald26 and Osborne23 considered these deposits along with numerous other titaniferous magnetite deposits in 1913 and 1928, respectively. None of these reports entailed a detailed study of the ore occurrence in this area. The present study was begun in 1940. Seven months were spent in the field, and considerable time was spent in labora-

Jan 1, 1949

By C. J. Osborn

In oral discussion at the Columbus midyear meeting, September 26, 1949, these pertinent questions were asked: Was a satisfactory separation of metal and matte obtained? The matte was quite fluid and in most cases the separation was satisfactory. Were the mattes chlorinated after aging? The mattes were stored in sealed glass mason jars, and chlorina-tion experiments made after standing for several weeks gave satisfactory results. Was ferric chloride volatilized? Most of the iron content of the matte was converted to ferric chloride. However, because of the low chlorination temperatures used (150" to 250°C) the major part of the ferric chloride remained with the residue. Undoubtedly, some ferrous chloride was also formed, because of the reducing conditions within the reaction vessel, but no effort was made to separate it from the ferric chloride. Could the reaction be stopped before making metallic iron? No attempt was ever made to stop the reaction before making metallic iron. Generally, 20 to 60 pct of the iron in the charge was obtained as metallic iron which could be readily separated from the matte. In certain cases, metallic iron was dispersed through the matte in the form of globules, which could be removed by magnetic separation. Could other sulphides, i.e., calcium sulphide or sodium sulphide be used in place of iron sulphide? No other sulphides were investigated. It was felt that titanates of calcium and sodium would be formed should these sulphides be used to replace the pyrite. What were the sulphur volatilization losses during matte smelting? In the course of this laboratory investigation, a rather wide variety of variables was introduced from highly oxidizing to reducing conditions and various ratios of pyrite, rutile, and coke. These and other factors all have a definite bearing on the sulphur losses. In general, the higher the sulphur in the charge the higher were the sulphur losses and the percentage of titanium in the matte decreased. With sulphur additions more nearly the theoretical amount, the sulphur losses averaged approximately 10 to 15 pct. With a higher percentage of sulphur on the charges, the losses were in the order of 15 to 30 pct.

Jan 1, 1951

The Secretary : The work of Mr. A. E. Outerbridge, Jr., of Philadelphia, first made known in his paper on " The Mobility of Molecules of Cast-Iron," read at the Pittsburgh Meeting of the Institute, in February, 1896, has been reviewed by the Committee on Science and the Arts of the Franklin Institute, whose report, dated May 5, 1897, is accompanied with a table of tests made by the Committee, and amply confirming the statements of Mr. Outerbridge. Concerning the originality and novelty of his investigation, the Committee says: " The fact that a certain molecular change takes place in cast-iron in the course of time has been known and recognized by many persons for a long time, and that this change tends to relieve the internal strains and render the casting tougher has often been noticed and acted on, although in a very crude way; but, so far as the sub-committee has been able to learn, Mr. Outerbridge has been the first to make a careful study of this, and to note that the change may be hastened by impact, and the whole effect produced in a short time, and also to make a scientific study of the phenomenon. We believe great credit is due him for the initial observation and the careful work dependent thereon. The results were first given to the public in a paper read before the American Institute of Mining Engineers, on February 20, 1896. This aroused a wide-spread interest and discussion among users of cast-iron, and so far as the sub-committee has been able to determine, it has not been shown that anyone, either in this country or abroad, has antedated Mr. Outerbridge in his work in this line. The Franklin Institute therefore recommends the award to him of the John Scott Legacy Premium and Medal." This report has not been published, hut I have had the opportunity to read it in manuscript. The table of testa accompanying it comprises 91 tests of " rumbled" and an equal number of " not rumbled" companion-bars of cast-iron, 26 by 2 by

Jan 1, 1898

By V. L., McCutchan

FORM of ore bodies, strength of wall rock, and quantity of water that must be handled differ so greatly in the various districts in which the Corporation operates that a variety of mining methods have to be employed. All are underground, however, with the exception of glory holes at Cerro de Pasco from which siliceous silver pacos ore is obtained. In general, the ors is in many relatively small bodies unsuitable for hulk mining, such as caving or top slicing. The strength of the rock and ore rarely permit open stopes, though shrinkage is successfully used on various veins with strong walls, particularly in, Casapalca. Horizontal cut and-fill and square-set stoping with careful filling are the principal methods employed, with the necessarily higher cost for supplies and labor offset as much as possible by care in the avoidance of dilution. The mines at both Morococha and Casapalca are notoriously wet, and even at Cerro de Pasco the quantity of water was enough to retard deep development until the perfection of electric pumps. In Morococha particularly, the extension of successive levels, first from adits of moderate length, then from shafts and heavy pumping installations on the 750 and 1000 levels, and finally by the 30,564-ft. Kingsmill tunnel, was one of the most difficult and long continued fights against water and resulting heavy ground that is recorded in mining history.

Jan 1, 1945

By I. Lowthian Bell

THERE has been probably no improvement introduced into the manufacture of iron which created more surprise in the minds of practical smelters and of scientific men than Neilson's discovery of the hot blast. In 1829, Messrs. Dunlop & Co. consumed at the Clyde Works, near Glasgow, nearly 7 3/4 tons of coal to make a ton of pig iron, of which about 20 cwts. was employed under the boilers of the blowing engines, leaving nearly 7 tons for the consumption of the furnace itself. In the year 1833, by heating the air to 612° F. (322° C.), they reduced the 7 3/4 tons to 3 tons by the mere burning of 8 cwts. of coal in the apparatus for raising the blast to this temperature. The statement just given is strictly true in a commercial sense, but when we come to consider the question as one of physical science, it is necessary to eliminate some of the conditions which conduced to so extraordinary a result. Anterior to Neilson's time the fuel employed in smelting iron was coke, and it was supposed at that period, erroneously, however, that coal in its raw state, when burned with cold air, was totally unfit for the purpose in question. This mineral, as it was obtained from the Lanarkshire coal-field, contained about 35 per cent. of volatile matter, but the process of charring it was performed in so unskilful a manner that instead of receiving 88 cwts. of coke from 135 cwts. of coal, 60 cwts. only was the product of the operation. Again, the reduced consumption of carbon in the furnace itself was accompanied by a corresponding diminution of blast, and this was followed by an economy of half a ton in engine coal. After making a proper allowance, however, for all these collateral circumstances, we are within the mark when we admit that in actual coke, which is really the form the fuel has to assume before it is burnt in the blast-furnace, not less than 30 cwts. was saved by heating the blast to 615° F. (322° C.). This unexpected economy, be it remembered, was obtained by the combustion of the 8 cwts. of coal, somewhat wastefully applied in the hot-air apparatus. Numerous have been the opinions advanced by different authorities in the scientific world to account for the apparent anomaly, but none,

Jan 1, 1877

By I. Lowthian Bell

THERE has been probably no improvement introduced into the manufacture of iron which created more surprise in the minds of practical smelters and of scientific men than Neilson's discovery of the hot blast. In 1829, Messrs. Dunlop & Co. consumed at the Clyde Works, near Glasgow, nearly 79 tons of coal to make a ton of pig iron, of which about 20 cwts. was employed under the boilers of the blowing engines, leaving nearly 7 tons for the consumption of the furnace itself. In the year 1833, by heating the air to 612' F. (322' C.), they redoccd the 79 tons to 3 tons by the mere burning of 8 cwts. of coal in the apparatus for raising the blast to this temperature. The statenlent just given is strictly true in a commercial sense, but when we come to consider the question as one of physical science, it is necessary to eliminate some of the conditions which conduced to so extraordinary a result. Anterior to Neilson's time the fuel employed in smelting iron was coke, and it was supposed at that period, erroneously, however, that coal in its raw state, when burned with cold air, was totsally unfit for the purpose in question. This mineral, as it was obtained from the Lanarkshire coal-field, contained about 35 per cent. of volatile matter, but the process of charring it was performed in so unskilful a manner that instead of receiving 88 cwts. of coke from 135 cwts. of coal, 60 cwts. only was the product of the operation. Again, the reduced colisumption of carbon in the furnace itself was accompanied by a corresponding diminution of blast, and this was followed by an economy of half a ton in engine coal. After making a proper allowance, however, for all these collateral circumstances, we are within the mark when we admit that in actual coke, which is really the form the fuel has to assume before it is burnt in the blast-furnace, not less than 30 cwts. was saved by heating the blast to 615° F. (322° C.). This unexpected economy, be it remembered, was obtained by the combustion of the 8 cwts. of coal, somewhat wastefully applied in the hot-air apparatus. Numerous have been the opirlions advanced by different authorities in the scientific world to account for the apparent anomaly, bat none,

By Cloyd M. Smith

A FEW years ago, the Ventilation Committee established the practice of presenting one topic each year for discussion at the annual meeting. The practice has met good response on the part of committee members and I suggest that it be continued. The topic chosen for this year, "Underground Anemometry," is a topic which has bothered me for more than 20 years. It seems to me that the coal industry is content to rely on slipshod methods for measuring the rate of flow of air underground, so I prefaced my discussional charge to committee members with the statement that I regard air measurements made in the usual way, with hand held anemometer, as no good. Agreements and disagreements came in from more than a dozen engineers, some of whom are with operating companies, coal and metal; some with manufacturers; others with government agencies.

Jan 1, 1949

By PHILIP N. MOORE

PHILIP NORTH MOORE was born on July 8, 1849, at Connersville, Ind. His father, a civil engineer, was descended from Henry Moore who came from Ireland in 1773 to live in Washington, Pa. Through his mother, Philip Moore was descended from John North, who came to America in 1635 and settled in Connecticut. The story of Mr. Moore's life as told by himself is given on pages 373-386 of T. A. Rickard's "Interviews with Mining Engineers." He studied at Miami University, where he gained the degree of A.B. in 1870, and A.M. in 1873. In 1920 his alma muter conferred on him the honorary degree of LL.D. He, as a special student, was a member of the class of 1872 at the School of Mines of Columbia University.

Jan 1, 1930

By Clyde E. Williams

IN planning a postwar program for manufactured products, it is essential that the bases for the plans be wisely chosen. First we must make certain assumptions as to the war's ending. Let us assume: (1) complete victory by the United Nations, (2) peace terms that will ensure the direction of the economy of all nations of the world toward peaceful pursuits, and (3) an early ending of the war, that is, before the nations of the world, excluding the enemy, are near the point of physical and spiritual exhaustion. Thus, our manufacturing plants and transportation facilities will still be in good shape. The plants and transportation facilities, as well as the cities of a large part of Europe, however, will be badly crippled. The rich mineral and other raw material resources of the world, little of which was under control. of the Axis powers before the war or will be after the war, will not be used up. Control of these raw materials, or at least an important part of them, will remain in the hands of the strong peaceful nations.

Jan 1, 1943

By John A. Gann

THE Iron and Steel Division has shared in the general increased activity of the industry. The fall meeting at Chicago was not only well attended but particularly characterized by the virility and scope of the discussions at the various sessions. The program for the February meeting indicates a similar interest in technological developments. The Blast-Furnace Committee continues to have the hearty support of the industry with discussions of such a nature as to be of real help to the operator as well ass the technologist. The work of the Open-Hearth Committee continues to be outstanding, with ever increasing attendance and ever mounting interest in the meetings. Formation of a conference on the physical chemistry of steelmaking has given those interested in this phase of work an organization allowing the same

Jan 1, 1936

By Robert T. Gdagher, Allison Butts

EDUCATIONAL trends as reflected in curricular changes are of interest and importance in engineering educa¬tion both as matters of record and as considerations for the future. The data on which the evidence of this report is based were obtained by sending questionnaires to all schools in the United States granting the undergraduate degree in mining engineering, metallurgy, or metallurgical engineering. The questionnaire had two parts, one inquiring as to the general nature of revisions made or planned, and the other asking for information on specific courses added to or dropped from the curriculum, or given more or less time than formerly. The frequency with which curricular changes are made, even in normal times, is notable. Although it was expected that the period since 1939-40 would show numerous revisions, it was somewhat surprising to find that of 62 mining or metallurgical curricula in existence in 1939-40 and reported in the present survey, 58 had been revised or are shortly to be revised, 52 having already been changed during this period. Moreover, approximately half of the mining schools that have already revised their curricula, and probably a similar proportion of the metallurgical schools, are about to make further important changes.

Jan 1, 1948

F. E. BACHMAN, Buffalo, N. Y. (Communication to the Secretary) : The investigation so fully described by Mr. Laudig was undertaken with the idea of determining if it is possible to learn by expesiment, without an actual trial in the furnace, what economical results can be expected from the use of a given ore-mixture. The research was necessarily preliminary, and the results obtained are only to be depended upon so far as they relate to the samples treated. With the exception of the ores obtained from the stock-piles of the Buffalo Furnace Company, and several samples taken at a neighboring furnace, there is no certainty that the ores represented the average shipments of any mine. For this reason the publication of the names of the ores might do producers a great injustice. The names of the ores arc therefore withheld, and their identity is further .veiled by leaving out of the analyses the phosphorus-contents. The investigation was begun with the preconceived idea that the rate of reduction would be found to be dependent upon the accessibility of the particles of the ore to the action of the reducing-gas. In other words, a spongy, brown hematite or a very fine Mesabi would be the easiest reduced. I had formed a scale with No. 21 first, No. 30 second, No. 1 third, Nos. 5, 24, 25 and the remaining Mesabis fourth, etc , which is sufficient to show how much actual results differ from a judgment based on physical characteristics. The ore expected to be most easily reduced proved to be 25th in the list, while the one placed

Jan 1, 1897

By E. P. Bayer

MESABI RANGE ore is mined largely by the open-pit method. This involves having available at all times sufficient working places which in combination will produce ore of guaranteed analysis. Fast- loading power shovels turn out under favorable conditions 1000 tons per hour from each unit. Each unit loads ore differing materially in analysis from that loaded by the others, One may load high grade, another low grade, and another may be in a mixed bank with the lead ore so placed that the product must be mixed at the shovel before it is loaded into cars. In such cases the bank is combed with the bucket, the door being left open to permit the material to fall through.

Jan 1, 1937

By H. C. Weed

THE Inspiration Consolidated Copper Co., located in the Globe-Miami district at Inspiration, Ariz., became a producer of copper in 1915. From 1915 until 1948, 116,278,000 tons of ore were produced from underground workings by the block-caving system of mining. In April 1948, open-pit ore production from portions of the ore body was started and earlier plans for block-caving in these areas were abandoned. The change was due to economic conditions.

Jan 8, 1950

By AIME AIME

AWRDED jointly by the four AW Founder Engineering Societies the John Fritz Medal is generally regarded as the most signal honor that American engineers can confer on a fellow engineer. The roll of 34 recipients contains the names of Lord Kelvin, George Westinghouse, Alexander Graham Bell, Thomas. A. Edison, George W. Goethals, Guglielmo Marconi, and Michael I. Pupin; and among members of the A.I.M.E. now living, Sir Robert A. Hadfield, Herbert Hoover, and Daniel C. Jackling. On the evening of March 1 7 the name of Paul Dyer Merica was formally added to this list of illustrious engineers when the medal was presented to him at a dinner at the Metropolitan Club in New York. The citation read. For important contributions to the development of alloys for industrial uses. Arrangements for the dinner were made by the following committee representing the four Founder Societies: R. C. Allen, George S. Davison, A. A. Potter, and J. B. Whitehead.

Jan 1, 1938

By Gordon E. Agar, David M. Hopstock

This paper describes the procedures and results of a series of experiments conducted to determine the depressing effect of sodium, calcium and magnesium ions on the amine flotation of quartz. It also presents an analysis of the experimental results by the electrical double layer theory. The flotation of quartz with primary amines has been practiced on a large scale in the phosphate industry for many years. Some glass sand —and recently iron ore — has also been treated by this flotation technique. These applications have been highly successful and demonstrate that a complete mastery of all the details of an operation is not needed to achieve an economic success. There are times, though, when it becomes important to recognize, both qualitatively and quantitatively, the effects of some previously ignored variables. The effects of cations on the amine flotation process, particularly those ions that contribute to water hardness and abound in sea water, are a case in point. In conjunction with the development of a cationic flotation reagent for separating quartz from apatite, it became necessary to quantify the influence of calcium and magnesium on the separation. In order to strengthen and broaden current understanding of the flotation process, the results were interpreted by means of the electrical double layer theory. THEORETICAL BACKGROUND Assume that, given the same equipment, procedure, and time, the recovery of quartz by amine flotation is a function of only the adsorption density of aminium ions in the Stern layer, i.e., that for any given adsorption density there exists only one recovery percentage. By the Stern-Grahame treatment of the electrical double layer,'-' for any ionic species in a solution in equilibrium with quartz,

Jan 1, 1969

By F. N. Rhines, W. S. Pellini

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245' to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247' to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250' to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By W. S. Pellini, F. N. Rhines

In many of the otherwise well established alloy phase diagrams the solidus curves (temperatures at which liquid first appears upon melting) have not been located accurately, chiefly because the experimental techniques that have been most popular for determining solidus temperatures have been both cumbersome and subject to large errors. C. E. Homer and H. Plummerl have described a sensitive and at the same time a very simple technique for locating the solidus curves in a number of alloys of tin. Their method consists simply in noting the temperature at which a specimen of the alloy ruptures under the influence of a light bending force. Although this method is not new, it has been little used for this purpose in the past; nevertheless, it appears so attractive in its possibilities of speed, simplicity, and precision that the investigations presently to be described were undertaken to verify its merits. The redetermination of the solidus and eutectic temperatures of the lead-antimony system was employed as a medium of experimentation. New values obtained in this way are believcd to be sufficiently precise to warrant a revision of the currently accepted lead-antimony phase diagram (Fig. I). Determinations of the solidus of the lead-rich lead-antimony alloy series have been published by X. S. Dean2 and by E. E. Schumacher and F. C. Nix. Their points are represented in Fig. I. In their work the solidus was not located at antimony collcentrations greater than 2 per cent; the curve was presumed to meet the eutectic horizontal at an antimony concentration of about 2.5 per cent. In the present studies the solidus has been traced to 3.5 per cent, where the eutectic horizontal is intersected (Table I and Fig. I). Within the range investigated by Dean and by Schumacher and Nix the agreement with their values is good. H. Seltz and B. De Witt,4 on the basis of activity measurements, have calculated that the intersection of the solidus and the eutectic reaction horizontal should lie at 3.86 per cent of antimony. The following determinations of the eutectic temperature have been reported: Roland-Gosselin,5 228°C.; Ewen,6 228OC.; J. E. Stead,7 24g°C.; Campbell,8 228°C.; W. Gontermann,9 245' to 252°C.; R. Loebe,lo 245°C.; E. Heyn and 0. Bauer,ll 245°C.; H. Endo,12 250°C.; R. S. Dean,= 247' to 258°C.; E. Abel, O. Redlich, and J. Adier,13 245°C.; W. Broniewski and L. Sliwowski,14 250' to 252°C.; H. Seltz and B. De Witt,4 25o°C. A temperature of 247°C. appears to have been generally accepted in recent years; it is the value most frequently obtained by the method of cooling curves. Values below 247°C. have usually been obtained by inferior cooling-curve techniques; those above 250°C., by the method of heating

Jan 1, 1943

By E. T. Turkdogan, M. T. Hepworth, R. P. Smith

The permeability of oxygen in 0 iron in the tempera-ture range 700" to 900 C and in 6 iron at 1450°C was determined by the rate of internal oxidation of iron, containing -0.1 pct Al. The solubility of oxygen in zone-refined iron was determined by equilibration with hydrogen-water vapor gas mixtures at 1450" and 1510°C; oxygen solubilities , for iron in equi1ibriu.rn with molten oxide, are found to be 66 and 83 ppm for these two temperatures, respectively. The diffusivity of oxygen in iron at 14500C3 as calculated from the permeability and solubility data, is (4.1 * 0.6) x 10 "B sq cm per sec. OXYGEN is one of the most common impurities present in iron or steel, mainly in the form of oxide inclusions. In the study of many metallurgical problems concerning solid iron, it is often desirable to know with a reasonable accuracy the solubility and diffusivity of oxygen over a wide temperature range. The solubility of oxygen in solid iron has been the subject of numerous studies yielding highly discordant results as seen for example from the literature surveys made by Meijering &apos; and Schenck et a1.&apos; As shown by Kitchener et aL3 and by Sifferlen, the high oxygen solubilities reported by many investigators are the result of oxidizable impurities which are often present in iron. In addition, there have been experimental problems associated with icaccuracy of oxygen analysis of iron containing less than 100 ppm 0. A number of studies have been made on the permeability of oxygen in a and y iron using Fe-Si, Fe-Mn, and Fe-A1 alloys in the internal-oxidation experiments.1&apos;2&apos;5&apos;6 However, no direct measurements have been made of the diffusivity of oxygen in iron. In the present work two sets of experimental measurements were made: permeability and solubility studies at 1450" and 1510°C and permeability studies only in the range 700 to 900°C. In both sets of permeability measurements slab-shaped specimens containing small predetermined amounts of aluminum in solution were exposed at constant temperature to gas mixtures of hydrogen, water vapor, and argon for varying times. These specimens were quenched, sectioned, and examined for oxygen penetration by metallographic observation of aluminum oxide particles which formed. From these data, it is possible to calculate the ratio of the diffusivity of oxygen in iron, D, to the equilibrium constant K for the reaction Hz(g) * O (dissolved in iron) = H,O(g). EXPERIMENTAL Permeability Measurements at 1450°C. An ingot of vacuum-carbon deoxidized iron containing 0.086 pct A1 was prepared, using commercial "Type lO4A Plas-tiron"; after hot rolling, specimens were machined into slabs a by 2 by 2 in. The impurity contents were: S, P < 0.002 pct; C, Mn < 0.01 pct; each of all other Usual impurities < 0.004 pet. The amount of oxide inclusions in this material, determined by a bromine-methyl acetate extraction, corresponded to about 20 ppm 0 in the iron which agreed well with the results of vacuum-fusion analysis. Each specimen was annealed at 1450°C for 1 hr in purified hydrogen, polished to a smooth surface, and then introduced into a controlled oxidizing atmosphere in a recrystallized alumina tube at 1450°C. The constant temperature zone (*3"C) was about 3 in. in length. The gas composition was controlled by mixing argon with hydrogen (using calibrated constant-head flow meters) and passing the mixture through a column of a mixture of oxalic acid dihydrate and 10 pct anhydrous oxalic acid, to establish a required water-vapor content in the gas mixture. The temperature of the oxalic acid dihydrate column was controlled by a thermostat. The total gas flow was in the range 800 to 1000 cu cm per min. The exit gas from the reaction tube was passed through a weighing bottle containing a desiccant, to cross-check the degree of water-vapor saturation, which for all experiments was about 97 pct of those derived from the data of Baxter and Lansing.1 For a typical experiment, a specimen was introduced into the furnace in a stream of dry argon and hydrogen. The specimen was then rapidly raised by a Pt-Rh alloy wire into the hot zone and allowed to reach the reaction temperature, at which time the oxidizing gas mixture was introduced. The oxygen potentials employed were sufficient to oxidize aluminum but not to cause liquid iron oxide to form. After a specified time, the experiment was ended by dropping the specimen onto a water-cooled copper block at the bottom of the reaction tube. The depth of the internally oxidized zone, hereafter called the "case", was determined by sectioning the specimen at right angles to the long direction. The section was then examined under a microscope equipped with a micrometer stage. In general, the oxide particles were fairly uniform in size and distribution, forming a reasonably well-defined interface between the oxidized and unoxidized region. A typical cross section as observed at X30 is shown in Fig. 1. A thermal macroetch was used in one selected specimen to delineate the case. A cross section of a previously oxidized slab was polished and reheated at 1450°C in a hydrogen atmosphere for about 10 min. Upon quenching, the surface relief shown in Fig. 2 was produced; causes of this effect are unknown. Permeability Measurements Below 900°C. A slightly

Jan 1, 1967