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By E. V. Potter, H. C. Lukens

The volume of hydrogen released from electrolytic manganese at various temperatures and pressures was determined in a previous investigation1 as part of a study to determine the most practical procedure for removing the hydrogen from electrolytic manganese metal. No attempt was made to determine the absolute volume of gas in the metal at any temperature and pressure; the volume of gas released showed only the variation in solubility with temperature and pressure. The results were very similar to those obtained by Sieverts and Moritz.² Both sets of data show a minimum solubility between 500' and 700°C., but they differ in certain respects; on cooling from 500°C., our results showed an increase in solubility of about 7 C.C. as compared with an increase of 34 C.C. per 100 grams shown by Sieverts. Furthermore, the transition temperatures, as indicated by sharp breaks in the solubility curves, did not agree well with Sieverts' data. This information was of secondary importance in the earlier investigations, and the solubility at low temperatures and the transition temperatures were subject to considerable error. Therefore, a subsequent investigation, reported in this paper, was made to measure the absolute solubility at temperatures from room temperature through the melting point and make more accurate observations of the transition temperatures. Apparatus and Method The apparatus and method were essentially the same as those described in the previous work,' as shown in Fig. I. At high temperatures, the small tube containing the thermocouple in the sample container A frequently broke off, so for some of this work the thermocouple was placed outside the sample container and protected by a quartz tube of about the same wall thickness as the sample container. No significant difference was found in the transition temperatures obtained in the two ways. The automatic temperature controller was used in these tests in the regions where there was little change in solubility with temperature. In the neighborhood of the transition points a continuously variable autotransformer was used instead of the automatic controller, and the power input to the furnace was adjusted so that the temperature increased or decreased at a very slow, uniform rate through the transition range. This procedure was followed because the temperature oscillations produced by the controller were too great compared with the transition range, and the transi- . tion points determined under such conditions were less accurate. Absolute Solubility Procedure ad Results The absolute solubility of hydrogen in manganese could be determined most

Jan 1, 1947

By W. D. Sylwestrowicz

In tests on polycrystalline copper and aluminum, the ratio of the yield stress to modulus of elasticity was found to be strongly dependent on tempemture. Also, it was shown that the change of the yield stress with temperature of a material at a given temperature and deformed to a given yield stress, but not necessarily to the same strain, does not depend on previous mechanical thermal history. Likewise, for a material at a given temperature and deformed to a given yield stress, the rate of work hardening is independent of the temperature of prior stressing. It has been shown by Los and Orowan1 and by Dorn, Goldberg, and Tietz2 that the temperature dependence of the yield stress-strain curves of crystalline materials reflects two effects: not only does the yield stress of a material in a given structural state depend on the temperature, but the structural state (and the corresponding strain hardening) after a given amount of plastic straining also depends on the temperature at which the pre-straining has been carried out. Thus, for instance, if a specimen of a ductile metal has been strained along the stress-strain curve 1 at room temperature to point A, Fig. 1, and then the straining continued in liquid nitrogen along curve NR, the yield stress A' immediately after lowering the temperature is lower than the yield stress A" of a specimen that has been strained by the same amount in liquid nitrogen (along curve 3). AA' represents the effect of the temperature change upon the yield stress of the specimen pre-strained at room temperature; A' A" is the excess strain hardening acquired if the pre-straining has been carried out in liquid nitrogen instead of at room temperature. The dependence of the yield stress (i.e., of the structural state acquired during preceding straining) upon the conditions (speed, temperature) of a pre-straining is the reason for the nonexistence of a so-called "mechanical equation of state" for plastic deformation. A 'mechanical equation of state" is a relationship of the form F(s,E, e, T) = 0, or s = f(E, E, T) [1] It was first suggested by Ludwik3 that plastic deformation might obey such an equation; this, however, was conclusively disproved by experiments of Kochendorfer.4 Additional disproofs were given in

Jan 1, 1959

By E. H. Jr. Dix

THE importance of aluminum-silicon alloys in the light alloy field is now generally recognized. Where silicon was once considered detrimental to the properties of aluminum, useful alloys now contain as much as 13 per cent. Furthermore, silicon is present as an impurity in aluminum of even the purest grades. Iron is another important impurity in aluminum and like silicon is found in small quantities in the purest aluminum available today. The manner of occurrence of iron and silicon in commercially pure aluminum and many of its alloys exerts, a very pronounced influence upon their properties. The effect of large quantities of iron in aluminum-silicon alloys is so detrimental that it has been found necessary to limit the allowable maximum percentage to as low a figure as is consistent with quantity production and satisfactory physical properties. The intimate relation existing between iron and silicon in aluminum and aluminum alloys makes necessary a more complete knowledge of this ternary system. This paper is divided into two principal parts, dealing respectively with aluminum-silicon solubility equilibria and the constitution of aluminum-iron-silicon alloys.

Jan 1, 1927

By C. A. Zapffe, C.E. Sims

Many hundreds of publications have appeared during the past 78 years that treat the subject of hydrogen in iron and steel.l05 but conclusions regarding the functions of hydrogen in causing some important defects in steel are still unsatisfactory to many; and other hydrogen-caused phenomena yet remain to be identified with this gas. The most widely discussed of these defects is hydrogen embrittlement, but the conception, perhaps the popular one, that embrittlelnent is due to hydride formation aoes not conform to the known facts.l04 The true identity of hydrogen embrittlement seems instead to lie in a mosaic nature of metal crystals, which is a concept not Yet accepted by most metallurgists. A study of hydrogen embrittlement therefore provides new viewpoints in regard to the crystalline substructure of steel.

Jan 1, 1941

By C. E. Sims, C. A. Zapffe

Many hundreds of publications have appeared during the past 78 years that treat the subject of hydrogen in iron and steel.l05 but conclusions regarding the functions of hydrogen in causing some important defects in steel are still unsatisfactory to many; and other hydrogen-caused phenomena yet remain to be identified with this gas. The most widely discussed of these defects is hydrogen embrittlement, but the conception, perhaps the popular one, that embrittlelnent is due to hydride formation aoes not conform to the known facts.l04 The true identity of hydrogen embrittlement seems instead to lie in a mosaic nature of metal crystals, which is a concept not Yet accepted by most metallurgists. A study of hydrogen embrittlement therefore provides new viewpoints in regard to the crystalline substructure of steel.

Jan 1, 1941

By Oliver Bowles

ROCK is no doubt the most abundant of all material things because the planet on which we live is made of it. All animal and vegetable organisms and the multitude of natural and manufactured products that occupy a comparatively insignificant film on the outer surface of the planet are derived from rock. Processes of Nature acting for untold centuries have transformed rock into soil, making possible the development of vegetable and annual life; and rocks have supplied the numerous raw materials, metallic and nonmetallic, wherewith the innumerable appurtenances of a complex civilization have been fabricated. As time goes on we live with increasing speed and with enlarged desires. Time and space are shortened by man's ingenuity, and products for human use must be manufactured with greater and greater celerity. It was inevitable that Nature's slow processes of rock alteration should fail to keep pace with human demands and that the variety of natural products should fall far short of the requirements of an industrial age. Man therefore supplemented these processes by attacking rock in its native bed amid using it to supply needs not otherwise satisfied.

Jan 1, 1934

By Robert M. Grogan, Gill Montgomery

Fluorspar, the commercial name for fluorite, is a mineral composed of calcium fluoride, CaF,. Its valuable properties are due to its content of fluorine, and it is the principal commercial source of that element. The name is derived from the Latin word "fluere," to flow, because the mineral has a low melting point and is used in metallurgy as a flux. Cryolite is a sodium aluminum fluoride, Na,AlF,. It is a rare mineral which has been found in commercial quantities in only one place in the world, Greenland. Small amounts of it are shipped from stock in that country, and its place in industry has been taken over almost completely by synthetic cryolite. Because of the relative unimportance of cryolite, discussion of it has been relegated to a short section at the end of this chapter, which is principally concerned with fluorspar. History Fluorspar was used for ornamental purposes by the Greeks and Romans, who fashioned such things as vases, drinking cups, and table tops from it. Various peoples including the Chinese and the American Indians carved ornaments and figurines from large crystals. Its usefulness as a flux was known to Agricola (1564), who wrote about it in 1546. Mining began in England about 1775 and at various places in the United States during the period 1820 to 1840. Production became substantial following the development and widespread adoption of the basic open hearth method of making steel, in which fluorspar is used as a flux. After that, production and usage were stimulated by growth in the steel, aluminum, chemical, and ceramic industries and were accelerated by World Wars I and II. Fluorocarbons entered the picture in 193 1 and the use of anhydrous hydrogen fluoride (HF) as a catalyst in the manufacture of alkylate for high octane fuel blends began in 1942. The development of the froth flotation process in the late 1920s, a differential flotation scheme for separating fluorspar from galena, sphalerite, and common gangue minerals in the 1930s, and the application of heavy-media concentrating methods to the treatment of low grade ores in the 1940s were outstanding technological contributions that enabled increased production of fluorspar concentrates. In recent years the development of pelletizing and briquetting processes for making flotation concentrates into gravel-size particles for use in steel furnaces and the development of more efficient and selective flotation schemes for treating crude ores containing abundant dolomite and barite have been major improvements in the industry.

Jan 1, 1975

By John Birkinbine

Through the partiality of my fellow-members I have been able, during seven years' service on the Council of the American Institute of Mining Engineers, to note the development of technical societies, a subject which commends itself as an appropriate theme for me, in retiring from the office of President, at a time when we meet in convention with Canadian technical societies. Our next assembly, called at Chicago at the time fixed for an International Engineering Congress, offers additional reason for the selection of this topic. If subsequent statements appear to give to the American Institute of Mining Engineers greater prominence than to kindred organizations, they may be excused upon the ground of long association with and loyalty to its members, and to a personal knowledge of their work. Besides, data as to its growth and development are more accessible; and at a meeting of the Institute features connected with it may be considered as of greater immediate interest than those affecting other organizations. The purpose of this address is, however, to use the record of the Institute as indicating a similar development of other technical societies, rather than to claim preeminence for any organization; the work of each must speak for it. There is a general tendency to form associations at the present time. Organizations have been created and are active in every profession and in all branches of labor, trade, industry, commerce, manufactures, science and art. A record of such associations and their aggregate membership would be startling, and would show how large a percentage of the population of North America is connected with one or more of them; but the figures cannot be even approximately estimated. The class of associations representing national, state, or local trade interests, such as boards of trade, chambers of commerce, etc., may be used as an illustration. A late report shows that in the

Jan 1, 1893

By Robert M. Grogan, James C. Bradbury

The Illinois-Kentucky mining district has, since 1880, accounted for 80 per cent of all U.S. production of fluorspar. The ore deposits are of two types: vein deposits formed by fissure fillings along faults and bedding-replacement deposits formed by the replacement of strata at certain favored stratigraphic positions along minor faults and fractures. Fluorite is the chief valuable mineral in the deposits. Sphalerite and galena commonly are present in small amounts but, in some ore bodies, may form a substantial part of the valuable constituents of the ore. Calcite is the chief gangue mineral; quartz and barite Exposed strata range from Devonian are present in various amounts. through Pennsylvanian in age. Igneous intrusive rocks occur as mafic dikes and sills and intrusive breccia dikes and plugs. Structurally, the district is situated on a generally northwest- trending arch that has been sliced into a series of long, narrow blocks by normal faults that trend northeastward. The structural The localization of the ore deposits by faults and fractures, the association of fluorite mineralization with intrusive breccias, and various lines of petrographic and geochemical evidence indicate that the fluorite-zinc-lead deposits were epigenetic and deposited by solutions emanating from a deep alkalic magma.

Jan 1, 1968

By E. V. Kleber, V. F. Novy, R. C. Vickery

The constitutional diagram for the gadolinium-cobalt system has been determined. Seven intermetallic compounds have been found at compositions corresponding to the follwing gadolinium-cobalt ratios: 3:1, 1:1, 2:3, 1:2, 1:3, 1:4, 1:5. The GdCor compound has a congruent melting point above 1600°C. whereas the remaining compounds melt incongruently. Eutectics exist at 16 wt pct Co and 84 wt pct Co, with melting points of 620° and 1260°C, respectively. PREVIOUS papers'" have recorded constitutional data for systems of gadolinium with iron and nickel. This paper presents data obtained on alloys of gadolinium with the remaining 3d transition element-cobalt. voge13 found that cerium forms, with cobalt, the intermetallic compounds; Ce3Co, CeCo, CeCo2, CeCo3, CeCo4, and CeCo5 Other workers4-' found the 1:2 compound in this series to exist in a C-15 (face-centered cubic) structure and the 1:5 compound to exist in a hexagonal crystal system. Comparison of earlier data with that now reported will be made subsequently. EXPERIMENTAL Methods of alloy preparation, annealing procedures, and experimental techniques have been previously reported.' The cobalt content of alloy specimens was determined volumetrically. RESULTS Microstructure—The alloy containing 10.5 wt pct Co corresponds closely to the composition of the first intermetallic compound Gd3CO. In Fig. 1 the microstructure is essentially single phase composed of Gd3Co which formed peritectically. The globular areas are remnants of the peritectic reaction which did not quite go to completion. A eutectic occurs between Gd3Co and the next higher compound GdCO, which is followed by a series of peritectic compounds. Fig. 2, an arc-cast alloy containing 20.2 wt pct Co, shows large primary crystals of GdCo etching either white or black (depending on crystallographic orientation), embedded in the eutectic. Similarly, in Fig. 3 at 31.2 wt pct Co, a compound, probably GdCo3, has separated from the melt. Subsequent peritectic reactions were almost completely by-passed as the alloy cooled, the residual liquid freezing as a fine eutectic. In the 47.5 wt pct Co alloy, Fig. 4, the high melting point compound, GdCO4, has solidified as massive, white-etching grains, which reacted with the liquid to form GdCo3 as the second phase. The microstructure of an arc-melted alloy containing 60.5 pct Co is complex, Fig. 5, and presents some difficulty in interpretation. The grey etching matrix is probably primary GdCO4. The dappled phase represents grains of GdCO5 which have separated from the melt on cooling. The discrete spots in this phase are eutectic liquid. Small light etching crystallites are probably GdCO5 formed by the incomplete high-temperature peritectic reaction. GdCO4 is retained in arc-melted specimens containing 70.5 wt pct Co, Fig. 6. White areas of this compound are held in a matrix of GdCO5 the appearance of which is mottled slightly by inclusions of the second eutectic in this system. The development of the spheroidized eutectic at high cobalt contents is depicted in Fig. 7 (80.3 wt pct Co) in which the white massive crystals are GdCO5 compound. Further development of this eutectic is seen in Fig. 8, the primary white phase here being pure cobalt. Thermal Studies—Differential thermal analyses and melting point determinations have yielded the data shown in Fig. 10. The high gadolinium eutectic, indicated by microscopy, was confirmed at about 16 wt pct Co, melting at 620°C . A eutectic also occurs at about 84 wt pct Co melting at about 1260°C. The thermal arrests at 8803 960°, 1060; and 1210°C,

Jan 1, 1962

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 Walter V. Knopp, Laurence Delisle

The aim of this work was the preparation of nickel-steels from elemental metal powders by powder metallurgy techniques. It was known that plain carbon steels could be made from a mixtufe of iron powder and graphite and that the effect of carbon on iron in powder form was of the same nature as that produced in fusion metallurgy. The problem in making nickel steels from elemental powders consisted therefore in finding out whether sufficient diffusion of the nickel and other incidental metals . normally present in such steels could be induced in the solid state to modify the properties of plain carbon steels made from powders and produce the beneficial effect of alloying. The composition selected originally was that of an S.A.E. 2330 steel. Metal powders, in the proportion correspending to that composition, were mixed with graphite, pressed, and heated at different temperatures for different periods of time, to produce bonding of the metal particles and mutual diffusion of the various elements without melting. Temperatures up to 1325°C and sintering periods as long as 6 hr were first investigated because it was expected.that such conditions would produce maximum diffusion with an accompanying improvement in the properties of the alloy. It was found that, although diffusion proceeded to a large extent under the conditions investigated, it would not be complete unless sintering were carried out at a high temperature for much longer than 6 hr. Relatively high temperatures and long sintering times are objectionable from a practical point of view, particularly when a low COSt material is to be produced, because they necessitate the use of special, costly equipment. Work could be done to improve the diffusion of iron and nickel by changing conditions other than the sintering temperature and time, that is, finer primary or alloy powders could be used. However, a marked change in the properties of the steel had been observed even with only partial diffusion. It was thought, therefore, that instead of trying to improve the diffusion, advantage might be taken of its incompleteness to produce a special structure consisting, in the unquenched condition, of a hard constituent, rich in nickel, dispersed in a tough pearlitic matrix. Steels with such a structure, not readily obtainable by fusion, should have desirable mechanical properties. Besides, it should be possible to prepare them from elemelltal powders under economical conditions. This latter alternative was therefore adopted for the second phase of this work. This report is divided into four parts: I. General Procedure. 2. Effect of Sintering Temperature. 3. Effect of Varying the Nickel Content. 4. Effect of Alloying Elements. General Procedure The general technique of cold pressing as used in powder metallurgy was applied.

Jan 1, 1949

By CLARENCE WM. POY

THE most common difficulty faced by an engineer or mine operator when opening a new property in a new field is the lack of roads and of cheap transportation. This one item often swings the balance of success or failure in starting a project. In Alaska, as elsewhere, such problems are more or less serious. In the boom days around the Valdez district, as well as in other parts of this territory, freighting was accom¬plished by dog teams or horses, or even by men that were willing to put their shoulders into harness, because there were virtually no roads. More important, there was only one time when supplies could be transported, and that was when there was suffi¬cient snow on the ground following a heavy wind. Then, and only then, could one depend on the snow to support horses and sleighs, and be sure that the gulleys, streams, and crevices in the glaciers were filled with snow to avoid pitfalls. These methods were used when one had no roads, no streams in the summer to float a barge, or even a trail for a pack train. If the snow was deep and soft, trans

Jan 1, 1935

By T. W. Beck

Roof bolter occupations in underground coal mines continue to experience overexposure to respirable dust. One potential source of dust in roof bolting operations is the exhaust from the roof bolter dust collection system. A wet exhaust conditioner (water box) has been developed to reduce dust emissions from the exhaust of the vacuum dust collection system on roof bolting machines. The exhaust conditioner consists of a muffler chamber and a water chamber with four internal partitions to direct airflow over the surface of the water. The National Institute for Occupational Safety and Health conducted a series of laboratory tests to assess the respirable dust capture ability of this device as compared to the standard exhaust muffler. To determine the dust collection efficiency, both devices were placed in the exhaust stream of a simulated roof bolter dust collection system. Gravimetric samplers were operated upstream and downstream of the exhaust conditioner and muffler to evaluate the ability to capture both respirable coal and limestone dust. Researchers observed a 41 % reduction in dust concentrations for the water exhaust conditioner in the laboratory configuration. Significant levels of dust deposition in the sampling chambers may have contributed to this effective capture rate.

Jan 1, 2012

By Henry S. Drinker

(Canal Zone Meeting, November, 1910.) FEW men reach middle life without having had the experience of failure in one or more undertakings; and most of us can look back with gratitude to help or advice given us by friends at critical periods of our lives. If, as men, we ask and take the benefit of such aid, why should we expect our sons to be stronger? A parent can make no greater mistake than to send a boy, however steady and intelligent he may be, off' to school or college, and expect the boy always to cope successfully with all the new conditions and new difficulties that may confront him. This is undoubtedly more the case with a freshman, in his first year at college, than in later years, or than it is with a boy at day- or boarding-school, where the boy receives a greater degree of care and oversight than can be given to the young man entering college; of all periods in life, the youth in his freshman year-fresh from the overshadowing care of home and school-may need judicious advice and timely aid. The change from the restraint of home and school to the freedom of college life is sudden and marked, and it is in this the first year of the boy or young man of 17, 18, or 19 years of age, that some tactful, judicious aid should be near him in his work and course. Some boys go to college so well prepared that they become careless and finally fall behind in their work from over-confidence. Others meet trouble from ambitiously trying to do more than their previous preparation, or physical or mental strength, can sustain. Others fall behind from illness-from injuries-from natural inability to grasp at first, without more aid than comes to them in the regular course of instruction, the higher mathematics-or mayhap the modern languages, or other subjects presented by the advanced curriculum of the present day. When a boy or youth begins to

Jan 1, 1911

By GEORGE ROBERT DE BEQUE

WHAT is wrong with oil shale? The answer is of interest to the public, to the oil refiner, and to the engineer. Many people have invested in shale land or shale securities, and others would invest if early development of the industry were certain. In the face of increasing demands for oil products, oil refiners are threatened with inability to maintain present output unless the supply of domestic petroleum is supplemented. Development of the oil shale industry would open a new field for engineering services. The object of this paper is to suggest reasons why there is but one shale plant in operation in the United States, and to discuss the probable time when the business will be firmly established in Colorado. As the Colorado deposits are the richest and largest in the world, ample supply of material is assured, consequently, this discussion will be confined principally to technical problems and economic problems affecting shale development.

Jan 1, 1924

By J. D. Hanawalt, W. H. Gross

Magnesium has long been known as the lightest of our engineering metals. This metal, silvery white in color, has a specific gravity of only 1.74. Aluminum, the next lightest structural metal, is 1 ½ times heavier; zinc is 4 times heavier; iron and steel are 4 ½ times heavier; and copper and nickel are 5 times heavier. Magnesium does not occur in the free state but is very abundant in nature, constituting 2.5 pct of the earth's crust in the form of various ores. It is the third most abundant structural metal, being exceeded only by iron and aluminum. Magnesium is unique, however, in that in the form of magnesium chloride it also exists in the oceans. Sea water is the source most widely used for production in the United States but magnesium is also commercially produced from magnesite, dolomite, and other ores as well as from certain inland brines. The vast quantity of magnesium existing in the waters of the oceans can be visualized when it is realized that the removal of one hundred million tons per year (the approximate annual steel production in the United States) for a million years would reduce the magnesium content of sea water only from 0.13 to 0.12 pct, providing no more magnesium had washed into the sea in the meantime. Not only is magnesium potentially very abundant but it is in addition a very versatile metal and can be shaped and worked by practically all methods known to the art of metal working. It can be cast by sand, die, and the various permanent-mold methods;

Jan 1, 1953

By Arne Bergholm

Australian rutile was chlorinated in the presence of CO or carbon. The chlorination velocity in CO was found to be strongly influenced by temperature and proportional to the CO concentration, but independent of the Cl, concentration. In the presence of carbon, the reaction velocity is much higher. The reactivity of the carbon and the distance between the carbon and the rutile surfaces are important variables. The reaction velocity is approximately proportional to the Cl, concentration and independent of the CO concentration of the surrounding atmosphere. Experiments with fluidized-bed chlorination of carbon-rutile mixtures indicate that the motion of the bed has little influence on the reaction velocity. At low temperatures, the chlorination velocity of dense tablets is much greater than that of TiO, coke mixtures suitable for fluidization. The reaction mechanism is discussed. In the industrial production of TiCl, rutile is chlorinated in the presence of carbon. Disregarding intermediate steps, the reaction may be expressed by the following equations: The ultimate object of this study was to find out whether the reaction velocity was higher in fluidized bed operation compared with chlorination of pelle-tized carbon-rutile mixtures. From a literature survey and preliminary experiments it was learned that some basic knowledge about the reaction mechanism was needed for a good experimental design. Therefore the following sets of experiments were carried out: 1) Studies on the reaction velocity in the chlorination of rutile with CO as the only reducing agent. 2) Chlorination of separate rutile-carbon tablets. 3) Chlorination of rutile-carbon tablets at different temperatures with various kinds of carbon, various grain sizes, and various tablet-making techniques. This series of experiments was carried out not only with pure chlorine but also with mixtures of chlorine with argon, CO and CO,. 4) Chlorination of rutile-carbon tablets made in a strictly standardized manner. 5) Chlorination of static-bed rutile-carbon mixtures. 6) Fluidized-bed chlorination of the same mixture. The experiments 4 to 6 formed the final and direct test of the main question: Static bed vs fluidized bedo. Although there are many patents and papers dealing with the general aspects of chlorination, only few experiments from which detailed information can be obtained have been reported in the literature. Pamfilov and coworkersl3 have studied chlorination of TiO, with CO or carbon as the reducing agent. They found that the weight decrease per hour at 600o to 800°C amounted to 11 to 14 pct with CO and 45 to 51 pct with carbon. They suggest that phosgene might be an intermediate in the chlorination of TiO,. Takimoto and Hattori have chlorinated reduced titanium oxide (TiO) and found a very high rate of TiC1, -production. They proved that the composition of the gas from the chlorination of rutile-carbon mixtures contained mainly CO. They reported for instance 74.7 pct CO, and 5.6 pct CO at 800°C at which temperature the Boudouard equilibrium composition is 12 pct CO and 88 pct CO. Seligman and Segerchano6 have studied the chlorination of TiO. They proved that Ti0 and chlorine react rather rapidly at temperatures as low as 300°C. Above 400°C, the reaction was complete. At 500°C the velocity of this reaction was much higher than was chlorination of TiO, + C. McTaggart,7 Nishimura, et al. and Wilskam have chlorinated mixtures of carbon and various kinds of rutile or beneficated ilmenite. Nishimura, et al. also report the results from reduction of TiO, with H2, CO, or carbon. At 900°C only 1 pct Ti O is formed in 2 hrs. At 1100°C 23.1 pct Ti, 0, was formed if elementary carbon was present. No carbide formation occurred below 1400°C. McIntosh and Cofferll have observed that the CO, content of the exit gases from chlorination of rutile and calcined petroleum coke is appreciably higher than found in the Boudouard equilibrium. At 900°C the ratio (CO, /CO + CO) is about 80 pct, whereas the equilibrium value is about 2 pct. W. E. Dunn12 has studied the chlorination rates of several TiO,-bearing minerals with CO + Cl, or COCl . Chlorinations were carried out either in a fluidized reactor or a fixed-bed reactor, both having a 30-mm diameter. The results obtained in both reactors were comparable. It was proved that benefi-ciated ilmenite (i.e., ilmenite from which the iron oxide had been removed by chlorination) was chlorinated 10 times faster thanrutile. Sore1 slag showed an intermediate rate. When phosgene is used, the

Jan 1, 1962

By P. Duwez, L. Zwell

L. S. BUSCH—We have had presented two methods of measuring these variations in powder compacts. E. OROWAN—Tn connection with the rolling mill research work carried out at. the Cavendish Laboratory, Cambridge, with the help of the British Iron and Steel Research Association. Dr. E. A. W. Hoff, Mr. J. Los, and myself, have determined coefficients of friction at ex- treme pressures for a number of liquid and solid lubricants, both by direct measurement, and by calculation from measured values of the roll force. The most efficient lubricants at these high pressures (for the small amounts of sliding that, occur in rolling) were camphor and. in particular, borneol (Borneo-camphor). Perhaps such lubricants could be used with advantage in the kind of work described by Dr. Wulff. L. S. BUSCH—1 think Dr. Wulff has in the past mentioned experiments which have been performed in the extrusion and rolling of metals and which led to conclusions which can be applied to the compacting of metal powder. A. SQUIRE*—There have been some recent developments in the field of high pressure lubricants which indicate that boron nitride might be a very desirable material to employ as a die lubricant. At the present time its cost is prohibitive, but as the need arises for the material it will undoubtedly come down in price. The present price is $200. a pound. It is my understanding that one of the reasons for vacuum pressing both in ceramics and metal powders, is to prevent

Jan 1, 1950

By Charles H. White

METHODS in colorimetry are based on the assumption that the intensity of the color of a definite volume of solution is directly proportional to the quantity of the color-producing substance' present. In the preparation and examination of colored solutions there are three ways in which the depth of color may be varied. These variables are; (1) the quantity of the coloring matter, (2) the quantity of the solvent, or the dilution, and (3) the thickness or depth of that portion of the solution examined. With these three variables as a basis, three general methods in colorimetry have been devised, all of which have been used in the determination of carbon in steel. In the first method, the quantity of the solution is kept the same for both the unknown steel and the standard, and the sections compared are of equal thickness, while the quantity of the standard is varied until the color obtained is of the same intensity as that produced by a definite quantity of the unknown steel. In laboratories where this method is used there is pre¬pared and kept for permanent use a series of solutions with varying amounts of the standard, representing the percentages of carbon from the lowest to the highest demanded in that laboratory. These standard solutions are kept in bottles, or test-tubes of equal diameter, and are arranged in series from the faintest to the most intense color, so that it is a simple matter to find the place of the unknown steel in the series, when the solution is of a definite volume and is contained in a tube of the same diameter as the standard tubes. In the second method, equal quantities of the standard and of the unknown steel are dissolved, the standard is diluted to a definite volume, and the solution of the unknown steel is di-

Sep 1, 1906