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By W. Rostoker, R. P. Elliott

TWO intermediate phases enter into equilibrium with the primary solid solutions of titanium.' The TiMn2 phase was identified by Wallbaum2 as of the C14 type isomorphous with MgZn2. Contrary to Maykuth, et al.,¹ the phase occuring at about the 50-50 atomic proportion has been shown to derive from a peritectoid reaction.:' A 30 day anneal at 900°C of an alloy containing 52 wt pct Mn developed sufficient of the new phase to give a clear and predominant diffraction pattern. The powder pattern was taken in a 14 cm diameter powder camera using filtered Cu Ka radiation. In all, 75 lines were recognized and measured. Interplanar spacing and observed intensities for the first 26 of these are given in Table I.

Jan 1, 1954

By Donald Barton

THE theory of gravitation is based on Newton's law that any two bodies exert a mutual attraction which is proportional to the product of their masses and inversely proportional to the square of the distance between them; i. e. A= K MM/R2 (1) where K is a constant, M and m are the respective masses of the two bodies, and R the distance between them. In the earth's gravitational system, the earth is one of the bodies; the other may be any body within or without the earth. In theoretical discussions and calculations in regard to gravity, that other body usually is taken as a unit of mass: in the C. G. S. system, a body of one gram in mass.

Jan 1, 1928

By Roger L. Beals, George A. Tweedy

I. INTRODUCTION. THE results of the cyanide-operations, given in detail in the following paper, show the progress that is being made at the Minas del Tajo. The old pan-amalgamation process, in operation up to and including 1905, while paying a profit on high-grade ores, was no longer able to treat profitably the ores in sight at that time, hence an alteration in the process was imperative. The success of this alteration is eloquently expressed by the following data Pan- Amalgamation. Cyanidation. 1905. 1907. 1903. Tons treated, . . 51,387 53,983 69,300 Value per ton (U. S. currency),. $10.75 $8.39 $8.28 Extraction, per cent., 65.00 88.50 S7.45 Extraction, per ton. .- $7.00 $7.4.; $7.24 Total cost, per ton treated, 6.50 4.311 4.01 Profit, per ton treated, . . 0.50 3.07 3.23.;

Feb 1, 1910

By Paul Billingsley

THE development of the North Lily ground, which lies in the East Tintic district, Utah,. about half a mile northwest of the famous Tintic Standard mine, was undertaken by the International Smelting Co. on purely geological reasoning. The geologic theory on which this work was based resulted from several years' intensive study of the East Tintic district by the geological department of the International Smelt-ing Co., who were, during this period, indebted to many for valuable suggestions that were adopted and became part, of the gradually maturing concept. For example, E. J. Raddatz, president of the Tintic Standard Mining Co., first called attention to the significance of rhyolite alteration; J. W. Wade, assistant manager, contributed greatly to our knowledge of the great Tintic Standard orebodies; and so on all along. the line. In short, the ultimate theory embodies the aggregate experience and thought of all those most familiar with the area in question. The problem in brief was this: is the Tintic Standard deposit an isolated occurrence of ore, or are other ore deposits to be found in the vicinity? If the latter is the case, where can these others be looked for? The difficulty of the problem lay in the fact that most of the area is covered by rhyolite; beneath which lies the limestone in which the orebodies occur; so that the available evidence as to the structure of the formations, and, their mineralization; is of the slightest. The sav-ing features of the case, by means of which it proved possible to solve the problem, are three in number first, the rhyolite is pre-mineral and hence has been exposed to alteration by the mineralizing agencies; second, certain persistent dikes and fissures are con-tinuous through the rhyolite into the limestone below; and third, the extensive underground workings of the Tintic Standard gave a good basis for study of the sub-rhyolite structure and the occurrence of ore. The rhyolite overlies the Tintic Standard orebodies, and over them shows a large patch of brownish altera-tion. This patch proves to be due to chloritization and sericitization, which has spread out from certain zones of dikes, pebble-dikes and fissures. The dikes are com-posed of a light fine-grained rock which has been altered to an aggregate of quartz, alunite, and magnetite. They can be traced southwest to a common center in Big Hill, the entire mass of which is composed of the same material. The pebble-dikes, which consist of a mass of rounded pebbles, mainly quartzite, in a matrix ranging from the same quartz-alunite-magnetite rock as above to almost pure vein quartz, are closely asso-ciated with these light dikes, but in general extend farther northeast. They thus represent a specialized phase of the intrusive action of which Big Hill is the center. The brown chloritized rhyolite, then, is an alteration product due, in all. probability, to emana-tions closely associated with this phase. Since it coin-cides geographically with the Tintic Standard area of highly altered limestone, with its many great ore-bodies, it has been concluded, that it is the expression in the rhyolite of activities which have also altered and mineralized' the underlying limestone.

Jan 4, 1927

By R. C. Troxell, S. C. Sun

EFFORTS to obtain definite quantitative data when employing the currently used bubble pick-up method1,2 as a pre-flotation investigation tool led to the adoption of the magnifying mirror method and the microscopic method modifications. Quantitative data obtained by these two methods were converted into bubble pick-up indices and bubble pick-up coefficients. Rough correlations were established between the calculated indices and the results of contact angle testing as well as actual flotation under the same conditions. The basic steps of the magnifying mirror method are as follows: 1—mixing 200 ml distilled water, sized and cleaned mineral particles of approximately 0.5 g, pH regulator, and flotation reagents in a glass beaker; 2—swirling the mineral particles to the center of the beaker to leave a clear circumference; 3—pressing an air bubble against the mineral particles for about 1 sec, and then moving the mineralized air bubble to the clear part of the beaker; and 4—dropping all the attached mineral particles of the air bubble by tapping the bubble holder, and counting the number of the dropped particles by looking at the magnified image in the mirror positioned beneath the beaker. This method is impractical for mineral particles which are transparent in water or finer than 200 mesh. The microscopic method is essentially similar to the above described magnifying mirror method, with the exception that the mineralized air bubble was drawn up into the bubble holder and subsequently discharged onto an externally placed watch glass, where the number of pick-up particles was counted with the aid of a microscope or hand lens. Drying was necessary when the discharged liquid interfered with the counting. The results of the bubble pick-up tests can be simply expressed in the form of the actual count. However, this can be misleading because the number of pick-up particles varies not only with the size of bubble but also with the size of particles. This short-coming is largely remedied by the use of the bubble pick-up index. as calculated from the following equation: PI = (pn/p) 100 [1] in which PI and pn are respectively the pick-up index and the number of pick-up particles under any test conditions, and p is the maximum number of pick-up particles of the same mineral under optimum flotation conditions, with the same size holder and particle. The bubble pick-up coefficient is a term coined to denote the difference between the bubble pick-up index of mineral particles in a liquid and that of the same mineral-liquid mixture plus a chemical reagent at the same pH value. For example, the difference between the pick-up index of a naturally floatable bituminous coal in a solution of water and kerosene and that of the same coal in water alone is a bubble pick-up coefficient. Compared with the contact angle method, the quantitative bubble pick-up method is inferior in accuracy but superior in sensitivity. Other advantages of the bubble pick-up method are that the apparatus can be easily assembled, the mineral sample is conventionally prepared, and the test procedure is relatively simple. References S. R. B. Cooke: The Flotation of Quartz Using Calcium Ion As Activator, Trans. AIME (1949) 184, p. 306. 'G. A. Last and M. A. Cook: Theory of Collector-Depressant Equilibrium at Mineral Surfaces. Paper presented at St. Louis Meeting, AIME (February, 1951).

Jan 1, 1954

By George F. Kunz

Jan 1, 1902

By F. W. Clark

At the present time, when lixiviation versus amalgamation is being so thoroughly discussed by practical men, and published information is so meagre, the following tests, made by students in the mining laboratory of the Massachusetts Institute of Technology, may be of interest to others. The ore experimented upon was obtained from the Sombrerete mines near Zacatecas, Mexico. A careful analysis of the dried sample resulted as follows : Per cent. SiO2,............62.79 S.............13.86 Al2O3............4.39 Fe,............11.26 Zn,............1.57 CaO.............2.91 MgO,........... 0.06 Cu,.............0.12 Pb,.............0.40 Sb and As,..........trace CO2,............2.35 Ag,.............0.16 99.87

Jan 1, 1886

By AIME AIME

FIVE days, extending from Monday, Feb. 18 to Friday, Feb. 22, inclusive, will be required for the annual meeting this year. The first fours days will be devoted to reading and discussion of papers, general and committee business meetings, two lectures, luncheons, dinners and all the pleasures of a big, general reunion. The fifth day will be given over to an all-day excursion for both men and women by special train to West Point, in celebration of the birthday of the first President of the United States. Washington having been an engineer and now after one hundred and thirty-one years the country having selected as President another engineer in the person of Herbert Hoover, our own past president and honorary member, it is proposed to celebrate with a good old-fashioned picnic and inspect the school. The authorities at the Military Academy have undertaken to welcome the engineers and do whatever they may to make our pilgrimage notable. Other social features planned for the week are numerous. Luncheon will be served as usual at the building each day of the meeting to all members and guests. This year a very nominal charge will be made, primarily to overcome deficits due to irregular attendance. Monday noon, the Non-metallic Minerals Committee will lunch at the Engineers' Club and in the evening the Milling Methods Committee will dine there. The Annual Smoker will be held at Hotel Astor after dinner. Professional entertainment of high order is promised, but not too much to interfere with the numerous group reunions that characterize this func- tion.

Jan 1, 1929

I-Mine Ventilation A. C. CALLEN, Chairman E. A. HGLBROOK, Vice-chairman H. I. SMITH, Secretary CLARENCE E. ABBOTT ALFRED W. HESSE FRANK H. PBOBERT GAM BRIGHT G. R. JACKSON GEORGE S. RICE THOMAS H. CLAGETT JAMES F. MCCARTHY E. J. RISTEDT . OSCAR A. GLASSER W. B. PLANK GERALD F. SHERMAN Coal Mining M. D. COOPER, Chairman HOWARD N. EAVENSON JOHN A. GARCIA THOMAS D. THOMAS CHARLES ENZIAN JAMES W. PAUL C. M. YOUNG JOHN J. RUTLEDGE

Jan 1, 1929

By Earnshaw Cook, H. S. Avery, J. A. Fellows

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. A. Fellows, Earnshaw Cook, H. S. Avery

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By DR. SAMUEL B. CHRISTY

? THE man is always greater than his work.? The training of the men who are to develop the mineral resources of the world is the most important problem connected with mining engineering. It becomes ever more important to civilization as the mineral wealth of the earth approaches exhaustion. I have therefore decided to consider a few of the more important problems arising in the training of the mining engineer, and especially those arising in America. THE PECULIAR NATURE OF MINERAL WEALTH. Mining and Agriculture are the two fundamental arts. Without the latter our existence would be precarious; without the former, our civilization impossible. Agriculture furnishes that regular supply of food and raiment which leads to the growth of large communities in which cultivated leisure first becomes possible; while raining furnishes the metallic thread from which is woven that complex fabric we call civilization. But in these two arts the conditions for success are widely different. Most of the crops that the farmer reaps may be harvested year after year, and the proper fertilizers being added, he may continue the annual harvest indefinitely, while, as a result of cultivation, his farm becomes yearly more valuable. But the crop the miner reaps can be harvested but once in the history of the race. Our mineral wealth has taken unknown ages to mature in the bosom of the earth. The ripened fruit can be plucked but once. There are no fertilizers for worked out mines. It never pays to work over a mine that has been

Sep 1, 1905

By Nestor Torres-Acuña, Fathi Habashi

Metallic copper of purity equal to commercial electrolytic copper is deposited during the anodic dissolution of technically available white metal, Cu2S, in m acidic solution of' copper(II) sulfate as electrolyte and copper sheets as cathodes. The process may be applied on commercial scale since it has the advantage of by passing the converting and poling steps, decreasing pollution problems due to SO, and recovering the sulfur of the white metal in the elemental form. The anodic dissolution is believed to take place in three steps: The working conditions that lead to 98 pct cathodic current efficiency are: 30 gpl Cu2+ and 100 gpl H2SO4 in electrolyte, current density 1.0 amp per sq dm, and tetnperature of bath 40°C'. DURING the smelting of copper, nickel, lead, and zinc sulfide ores, large amounts of sulfur dioxide are produced. Because the release of this gas in the atmosphere causes pollution problems, many attempts were made in the past for its recovery either in liquified form or processed to sulfuric acid. Although these two forms of sulfur are the usual forms that are consumed by the chemical and metallurgical industries, their storage and transport usually raise economic problems. It was realized, long ago, that a process by which sulfur can be recovered directly in the elemental form would be most attractive. Elemental sulfur is easily stored and transported, and is readily converted to SO2, H2S, or H2SO4 when needed. Processes aimed to recover the metals from their sulfide ores, and at the same time by-product sulfur in the elemental form, were recently reviewed.' As early as 1882, Marchese2 patented a process in which a matte having the composition: Cu 15, Pb 14, Fe 41, and S 25 pct was electrolyzed. According to cohen3 the process was applied on a pilot scale by the Aktiengesellschaft fur Bergbau-, Blei-, und Zinkhiitten-betriebe at Stolberg, Rheinland, Germany. The process was unsuccessful, however, owing to the contamination of the electrolyte during electrolysis. Studies in this field were reported by Bernfeld4 and Egli.5 Borchers et a1.6-8 developed the process further by using white metal (Cu 78.2 pct, S 19.6 pct) instead of the matte, and a pilot plant was operated by the Mansfeldschen Kupferschiefer Co. at Eisleben, German~.~ It appears, however, that the process never went into commercial operation. Further studies in this direction were carried out by Russian workers.10-23 The International Nickel Co. of Canada erected a pilot plant at Port Colborne in 1951 to apply the process to nickel matte which is essentially pure nickel sulfide."'- 26 Full-scale plant went into operation at the Thompson Refinery in Manitoba in 1964.27 In this method nickel sulfide matte is melted and cast into anodes analyzing 76 pct Ni and 20 pct S with small amounts of copper, cobalt, and iron. These anodes are then electrolyzed in an aqueous solution of NiS04 at pH 4. Further work on this method was reported in the literature.28-31 In this paper, experiments on the anodic dissolution of white metal in aqueous copper sulfate solution are reported. EXPERIMENTAL White metal, Table I, obtained from The Anaconda Co., was cast in form of anodes 10 by 7.5 by 1 cm, Fig. 1. The anodes are mechanically strong and do not break easily; when polished they gave a shiny gray metallic appearance. From the chemical composition shown in Table I, it can be seen that the atomic ratio Cu:S corresponds approximately to the formula CU2.06S. The copper in excess to the formula Cu2S is most probably present as a separate phase since metallic copper could be seen under the microscope, Fig. 2. Fig. 3 shows the X-ray diffraction pattern of white metal which matches fairly well with that of reagent-grade Cu2S.

Jan 1, 1969

By Grafton Thrasher

For the proper discussion of this subject it is necessary to incorporate in this paper the substance of part of an article published by rite in Metallurgical and Chemical Engineering for January, 1915. CAST-IRON TEST PLUG, SHOWING LOW MOTTLED AND MOTTLED FRACTURES. Several years ago, while I was thief chemist for a malleable-iron company, it occurred to me that the mere regulation of silicon was not sufficient to produce the desired degree of chill. But only after repeatedly encountering this fact in befit open-hearth and air-furnace, as well as cupola metal, was I led to regard variation in the total carbon as the principal cause of disturbance; and I resolved to determine the total carbon as well as the sill on ill every heat, and by a carefully prepared test piece to gauge the approximate degree of chill. The test piece selected was a round plug, 2 in. in diameter and 12 in. long, cast on end

Jan 10, 1915

By M. J. Sinnott

WITH the advent of nodular iron as an engineering material, considerable interest has been shown in developing this material for various applications. Generally the strength, hardness, or ductility are the more common properties used for design purposes but occasionally applications involving a knowledge of the thermal conductivity of the material is required. A search of the literature showed, rather surprisingly, that relatively little work has been done on this property for all types of cast iron. Insufficient data are available on thermal and electrical conductivities to develop the Weidemann-Franz ratio, or the Lorentz relationship, for estimation purposes. There are no data on nodular irons and the published data on malleable irons are quite sketchy. For these reasons the conductivity of the group of nodular irons listed in Table I were measured. Irons I to IV were made in such a fashion as to maintain the carbon and alloy content essentially the same while varying the silicon content. Test specimens were cut from the mid-section of 4-in. keel castings. Iron V is a commercial casting of nodular iron. The test specimen of this iron was cut from the center of a large cast billet 3x10x26 in. All alloys were tested in the as-cast condition. A microstructural examination showed that each iron had spheroidal graphite but the size and distribution varied with the silicon content of the iron. The spheroid size decreased while the number of graphite nodules increased as the silicon content of the iron was increased. The matrix structures of each iron consisted of pearlite and ferrite with the proportions varying from predominantly pearlite in the low-silicon iron to mostly ferrite in the high-silicon iron. The commercial heat, iron V, was predominantly pearlite probably because of its higher manganese and phosphorus content. Two methods for measuring the thermal conductivity were used. The first was a modification of the techniques described by Powell and Hickman and Van Dusen and Shelton,² the second method was a simpler technique described by Jakob and Hawkins." Since the agreement of both methods as tested on two sets of duplicate samples was excellent, the simpler experimental technique was used. The results of the measurements are given in Table II along with a summary of the microstructural constituents. These conductivity data indicate that as the percentage of silicon increases there is a corresponding decrease in the thermal conductivity even though the structure is changing from pearlitic to ferritic. Such a change in microstructure is usually accompanied by an increase in conductivity. A third factor involved in the behavior of these irons is the size and distribution of the graphite nodules. The relative amounts of graphite do not change greatly but the size and distribution do. Generally graphite improves the conductivity but in the present case such an effect is probably masked by the alloying effect from the silicon and its dispersion through the matrix. The thermal conductivity of the nodular irons studied is less than that of regular foundry irons by some 10 to 30 pct and is less than that of regular malleable irons.' The cause of the decreased conductivity is probably the more highly alloyed fer-rites obtained in these irons and the changed mode of distribution of the graphite as compared to the regular foundry irons. References R. W. Powell and M. J. Hickman: Journal Iron and Steel Inst. (1946) 154, No. 2, p. 99. 'M. S. Van Dusen and S. M. Shelton: U. S. Bur. Standards Journal of Research, RP668 (1934) 12, p. 429. ³M. Jakob and G. A. Hawkins: Elements of Heat Transfer and Insulation. 2nd Ed. (1950) New York. John Wiley and Sons. ' J. W. Donaldson: Journal Iron and Steel Inst. (1933) 128, No. 2, p. 255.

Jan 1, 1954

By U. N. Bhrany, N. Arbiter

F. C. Bond (Consulting Engineer, Processing Machin-Dept., AllisChalmers Manufacturing Co., Milwaukee) This is a very comprehensive paper. It deals with 1) size distribution functions, 2) energy-particle size relationships, and 3) criteria for grinding efficiency. The method of analysis used consists of tracing the increase and decrease of successive Tyler scale screen fractions as grinding progresses. The treatment is based upon the assumption that the work done in grinding is concentrated entirely upon the coarse size fractions in the mill. It is postulated that when a feed consisting entirely of particles of one size fraction is batch ground that finer fractions increase at a constant rate as grinding progresses, until finally each in turn begins to be ground and to decrease in amount. It is shown that under these conditions the empirical Gates-Gaudin-Schuhmann log-log size distribution plot can be logically explained. It is difficult to imagine any condition of ball mill operation, or any probability analysis, which would result in no grinding contacts on the finer particles present. However, the authors' postulate must be accepted if their conclusions are to be sustained. They conclude that the equation expressing the for mation rate of each size fraction can be resolved into the G.-G.-S. size distribution equation, and that the curvilinear portion of the log-logsize distribution line represents the only particle sizes which are being ground as well as produced. The author's statement that the G.-G.-S. Eq. 4 applies only to the finer portion of the size distribution while the Rosin-Rammler Eq. 6 applies over the whole size distribution range certainly supports the view that an exponential equation of the Rosin-Rammler type corresponds more closely to actual size distribution than does the power law G.-G.-S. equation. However, the G.-G.-S. equation is used to derive Eq. 8 and Eq. 9, which state that the energy required to grind a ton through a particular mesh varies inversely as the particle size to the exponent -a , whic h is the slope of the extended G.-G.-S straight line. This is stated to apply to both batch and continuous grinding. The G.-G.-S. slope exponent thus becomes very important in all crushing and grinding analyses by this method. The authors include some data which can be used to test their conclusions, as described below: We will consider grinding a feed composed of 14 mesh (1190u) to -200 mesh (74u). The average of 17 Allis-Chalmers grindability tests on quartz gives a work index (Wi) of 12.77. The -200 mesh product should have 80 pct passing 41.6u or P = 41.6. The equivalent 80 pct passing size of the 14 mesh feed particles is considered to be the particle diameter, as is true for spherical particles. Thus F is 1190u. In the work index equation 10 wi 10 wi 127.7 127.7 P f 41.6 1190 = 16.1 kw-hrperton. In Table I the ball mill exponent for quartz is 1.0 and from Eqs. 9 and 10: w=kw-hr/ton =Constan/(do/di) = 16.1 ton so that (1190) Constant/ Constant and the Constant equals 259. The tons per horsepower-hour value is 0.0464, in agreement with Table IV. The exponents for other minerals are listed in Tabl e 11. In Table IIA, the kilowatt hours per ton required to grind these minerals between the same sizes as the quartz, both by the authors' method and the work index equation, are listed. According to the authors kw-hrperton = 259/(16.1)".

Jan 1, 1961

By Willard L. Hunter

Four solvent extraction systems were studied to determine their efficiency jor extraction and separation of tantalum and columbium. Aqueous feed solutions of varying HF-HCl concentrations and metal content were contacted with equal volumes of cyclohexanone, 3-methyl-2-butanone, and 2-pentanone and solutions of varying HF-H2S04 concentrations were contacted with equal volumes of 2-pentanone. One multistage continuous test was made in a polyethylene pulse column using cy clohexanone as the organic phase. In each system studied, columbium and tantalum purities in excess of 95 pct with respect to each other were obtained in single-stage tests at low acidities in the feed solution. Separation factors ranging from 1700 to 2400 were obtained when rising HF-HCl mixtures in the aqueous phase. Best results were obtained when a solution of HF-H2S04 was used as the aqueous phase and 2-pentanone as the organic phase. A separation factor in excess of 6000 was obtained in one stage with aqueous solution concentrations of 2 _N HF and 2N H2S0,. When acid concentrations were increaszd to 52 HF and 10 _N H2S0,, 99.9 pct of the tantalum and 98.2 pct of the columbium initially present in the feed solution were transferred to the organic phase. The separation of columnbium and tantalum obtainable by means of the solvent extraction systems presented in this paper was found to corn -pare favorably with other systems, including the HF-H2SO4-methyl isobutyl ketone system currently used by most producers for the extraction and separation of these metals. TANTALUM and columbium are always found together in minerals of commercial significance, although the proportion of the two metals in ores varies within broad limits. Columbium is estimated to be 13 times more abundant than tantalum. Five methods generally employed for the separat:ion of these metals are: 1) fractional crystallization (the Marignac process),2 2) solvent separation, 3) fractional distillation of their chlorides, 4) ion exchange, and 5) selective reduction. Of these methods, the one currently used by industry to the greatest extent is that of solvent separation. One of the early technical developments in solvent separation of tantalum from columbium was reported by the Bureau of Mines: the HF-HC1-methyl isobutyl ketone system; data were presented for both laboratory and pilot-plant experimentation.3 Of twenty-eight organic solvents tested for their ability to extract tantalum from an HF-HC1 solution of columbium and tantalum, 3-pentanone (diethyl ke-tone), cyclohexanone, 2-pentanone, and 3-methyl-2-butanone were chosen for further study. Data on the HF-HC1-diethyl ketone system has been published4 and data describing the use of cy clohexanone, 2-pentanone, and 3-methyl-2-butanone as the organic phase are included in this report. RAW MATERIAL The source of tantalum and columbium oxides for this study was ('Geomines" tin slag from the Manono Smelter, Cie Geomines, Gelges, S.A., Congo. In order to extract the valuable Ta-Cb content, the slags were carbided, chlorinated, and the sublimate from chlo-rination was hydrolized and washed free of chloride with water. The washed material was air-dried and stored in a stoppered container. Throughout the paper, "feed material" refers to this mixture of hydrated oxides which was employed because of its high solubility in aqueous solutions. Typical analysis of the hydrated oxides is shown in Table I. I) HF-HC1-CYCLOHEXANONE SYSTEM Batch Separation. Effect of Acid Concentration. To determine the effect of varying the acid concentration upon the transfer of tantalum and columbium, a series of tests was made in which approximately 2.5 g of feed material was added to 25 ml solutions of 2, 4, 6, 8, and 10 N HF and 0 through 5 N HC1. Tantalum pentoxide concentration of the solu%ons was approximately 21 g per liter and columbium pentoxide was 14 g per liter. These starting solutions were shaken with equal volumes of cyclohexanone in 100 ml polyethylene bottles for 30 min. The phases were carefully separated in 125 ml glass separatory funnels. The time of contact of the solutions with the separatory funnels was kept at a minimum to reduce silica contamination. The measured phases were separated into 400 ml polyethylene beakers and the metal contents of each were precipitated by addition of an excess of ammonium hydroxide. Precipitate from each phase was filtered on ashless filter paper, ignited at 800" to 1000°C for 45 min, weighed, and analyzed by X-ray fluorescence.5 Data tabulated in Table I1 and illustrated in Fig. 1, show that maximum separation of tantalum from columbium for each HF concentration was obtained with no HCl present. The purest tantalum product was obtained with some HCl present. The highest separation factor was obtained at 2 N HF and

Jan 1, 1970

By R. M. Waterstrat, E. C. van Reuth

BINARY- alloy phases having the A15-type crystal structure have been described as occurring at a simple and more or less invariant stoichiometric composition (A3B) which corresponds to the relative number of atoms occupying each of the two crystallographi lattice sites in this structure.1,2 It is frequently assumed, therefore, that each crystallographic site is occupied exclusively by one kind of atom. In most cases, however, there have been insufficient experimental data to establish whether atomic ordering is, in fact, complete. Recent studies have shown that binary A15-type phases are sometimes stable over an appreciable composition range3''* and, occasionally, the composition range of stability does not even include the "ideal" A3B stoichiometric composition.5-7 We have observed the existence of nonstoichiometric A15-type phases in the binary systems Cr-Pt and Cr-Os. This has not been reported in previous work on these alloy systems.1,8-11 A series of alloys, each weighing approximately 30 g, was prepared by are-melting in an Ar-He atmosphere using 99.999 pct Cr, 99.999 pct Os, and 99.99 pct Pt as starting materials. Each alloy was melted four times with a total weight loss of less than 1 pct. The stoichiometric (A3B) alloys were sealed in evacuated quartz tubes and annealed at 1200°C for periods of time ranging from 3 days to 2 months. Examination of the alloy microstructures revealed that little change had occurred over this time interval and it was therefore assumed that the microstructures were fairly representative of equilibrium conditions. No evidence of contamination was observed although there was apparently some loss of chromium which was confined to a thin layer at the surface of the specimens. The quartz tubes were quenched from the annealing temperature into cold water. X-ray diffraction and metallographic examination of the stoichiometric alloys revealed an estimated 10 to 30 pct of second phases which were tentatively identified as phases previously reported in these binary-alloy systems.8-11 A second series of alloys was prepared by mixing -325 mesh metal powders having a nominal purity of 99.9 pct and compressing these mixed powders in a cylindrical die at a pressure of 43,000 psi. These alloys, each weighing 15 g, and some of the arc-melted alloys were annealed in a high-temperature vacuum furnace heated by tantalum strips at a pressure of 10-8 Torr and were rapidly cooled by turning off the furnace power. X-ray and metallographic examination of both series of alloys served to establish the composition ranges of the A15-type phases. Although some chromium losses occurred during the vacuum annealing, they were largely confined to a thin layer on the outer surfaces of the samples. It was established that the A15 phases occur in the Cr-Pt system at 21 ± 1 at. pct Pt after 1 week at 1200°C and in the Cr-Os system at 28 ± 1 at. pctOs after 1 day at 1400°C (see Table I). We also observed that an arc-melted stoichiometric (A3B) alloy in the Cr-Ir system was single-phase (A15-type) in the "as-cast" condition in agreement with previous work.8,13 In addition we obtained a sample of the Cr-Os A15-type phase from Argonne National Laboratory. This alloy contained less than 1 pct second phase12 and was submitted to a density measurement. The density measurement yielded a value of 11.14 g per cu cm in comparison to a theoretical value of 11.25 g per cu cm calculated using the observed lattice constant (4.6806Å) of this alloy. The uncertainty in measurement was 0.1 pct but the sample may have contained some cracks or minor imperfections which could account for the low experimental value. We have also studied the atomic ordering in these phases by means of integrated line intensity measurements using thick, flat, rotating powder samples and CuK a radiation in an X-ray diffractometer. We have obtained order parameters of 0.90 for the Cr-Pt phase, 0.89 for the Cr-Ir phase, and 0.64 for the Cr-Os phase using the formula: where s is the usual Bragg and Williams order parameter, ra is the fraction of chromium atoms in A sites, and FA is the fraction of chromium atoms in the alloy. The values obtained are estimated to be accurate within ±4 pct. If the unusually small value for the order parameter of the Cr-Os A15 phase were due to the existence of lattice vacancies on the "B-atom" sites, then a density of 10.04 g per cu cm would be expected in contrast to the observed value of 11.14 g per cu cm. We, therefore. conclude that the fraction of lattice vacan-

Jan 1, 1967

By D. J. Mack, R. E. Reiswig

Six examples of the peritectoid transformation were selected from the literature and studied by the method of isothermal transformation. The kinetics and mechanisms of five of the examples are presented as TTT diagrams and photomicrographs. The exist-enc- of a peritectoid in the sixth case is doubtful. ALTHOUGH the peritectoid transformation per se has been known for many years, no precise published data exist concerning the kinetics or mechanisms involved in transformations of this type, except for the brief treatment by Rhines, et al. 1,10 Bearing in mind the fact that investigations of recent years are uncovering more and more peritectoids and suspected peritectoids, a thorough study of the well-established peritectoids appeared to be in order. It was for this reason that a study of the kinetics and morphological mechanisms of six binary peritectoids was undertaken. The six peritectoids selected from the literature for study were those reported at 7.02 wt pct Al-Ag, 26.0 wt pct Sb-Cu, 30.5 wt pct Sb-Cu, 32.3 wt pct Sn-Cu, 8.35 wt pct Si-Cu, and 21.2 wt pct Al-Cu. These selections were based on availability and purity of components, ease of preparation and heat-treatment, and estimated reliability of the available equilibrium diagrams in the regions of interest. EXPERIMENTAL PROCEDURE The alloys used in this investigation were induction melted in electrode-grade graphite and chill-cast in cast-iron split molds. In all cases, the alloys were so brittle that they could easily be broken into samples weighing 1 or 2 g. Chemical analyses showed that the alloys used were close to the respective peritectoid compositions reported in the literature and that the impurity levels were low in all cases. Metallographic examination showed uniform distributions of phases in all samples, indicating uniformity of composition in the samples studied. Isothermal transformation studies were carried out in fused-salt media, using the familiar inter-rupted-quench method. Uniformity of temperature in the salt baths was maintained by continuous stirring with a stainless-steel agitator. On the basis of actual observations of the temperature fluctuations, the estimated temperature control was + 10C for the Ag-Al and Cu-Sb alloys and ±30C for the Cu-Sn, Cu-Si, and Cu-Al alloys. The accuracy of all temperature measurements was estimated to be ±1°C. It was found necessary to mount metallographic specimens of the Ag-Al alloy in cold-curing methyl methacrylate, since the temperatures encountered in mounting in bakelite or lucite caused an appreciable degree of transformation to the ß phase. For the other alloys, wood-flour-filled bakelite mounts were used to avoid extraneous X-ray diffraction lines during the later examination of the metallographic specimens on a Norelco Geiger-counter d if f r ac tomete r. In the X-ray diffraction procedure, agreement between the published diffraction patterns and those obtained in this study was good. This was particularly important for phase identification, since the literature contained little in the way of micrograph description in some cases. Etching of the silver-aluminum alloy for metallographic examination was done by swabbing with either of the following reagents: 1) 10 g CrO3, 1 g (NH4), SO2, 0.5 g NH4NO3, 100 ml H2O, or 2) 10 ml NH4OH, 1 ml 20 pct KOH, 4 ml 3 pct H2O2, 5 ml H2O. The other alloys were etched with the usual bichromate etchant: 2 g K2Cr2O7, 1.5 g NaC1, 8 ml conc. H2SO4, 100 ml H20 (swabbed vigorously). EXPERIMENTAL RESULTS A) The Ag-Al peritectoid at 7.02 wt pct Al— The phase equilibrium involved in this peritectoid is shown in Fig. I.2 The phase boundaries in the vicinity of the peritectoid were most comprehensively established by Hume-Rothery, et al,3 who placed the equilibrium temperature at 448 °C and the equilibrium compositions of the a ß' and y phases at 6.11, 7.02, and 7.24 wt pct Al, respective The alloy used in this study analyzed4 6.95 wt pct A making it slightly hypoperitectoid according to the accepted equilibrium diagram. The rate of the transformation a+ y — ß' varies rapidly with degree of undercooling below the equilibrium temperature, passing through a maximum in the vicinity of 350°C. Thus the TTT dia-

Jan 1, 1960

By J. R. Long, R. S. Dean, F. S. Wartman, E. T. Hayes

The production of titanium in I5-lb. lots and with a purity sufficient to be consolidated into ductile metal, as described in a previous paper,' has provided adequate material for a study of the physical properties of titanium and a more thorough examination of its working qualities. Data on the physical properties reported in that paper were obtained on metal fabricated by a fixed procedure, standardized for the purpose of control of the reduction, and are representative only of material fabricated under those conditions. There are many possible variables in the working schedule, which will have significant effects on the properties of the finished material; and since the previous working methods were not necessarily the best, an investigation of the fabrication of titanium by other methods was undertaken. In this work the consolidation of the powder by pressing and sintering was conducted essentially as outlined in the report cited' and all efforts were centered on fabrication methods for those powders and the proper- ties produced by them. Hardness, density, microstructure, and tensile properties were determined at various stages in the working and annealing; and resistivity measurements were made on a few bars and drawn wire. Consolidation of the PowdeR The screen analysis of the available titanium powder is given in Table I. No attempt was made to alter the size distribution from that noted because this powder, although coarse by normal powder-metallurgy standards, produced acceptable compacts suitable for the present work. Because of their large specific surface, finer powders are more contaminated by oxygen and produce harder compacts, which are difficult to work. The powder as produced is soft, compresses in a normal fashion, and exhibits very little tendency to adhere to the die surfaces. Unlike aluminum and magnesium powders, it can be readily pressed without the use of die lubricants. When compacted at 50 tons per

Jan 1, 1946