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By Dale A. Vaughan, Oliver M. Stewart, Charles M. Schwartz

Solid-solubility limits at 1500°, l000q and 500°C for carbon, nitrogen, and oxygen in high-purity tantalum were determined by X-ray lattice-parameter methods. For carbon, the solubility was found to be 0.17 at. pct at 1500°C, and less than 0.07 at. pct at 1000°C. A nitrogen solubility of 3.70 at. pct at 1500° C decreases linearly with temperature to 2.75 at. pct at 1000°C, and 1.8 at. pct at 500°C. In the case of oxygen, the solubility was found to be 3.65 at. pct at 1500°C, 2.95 at. pct at 1000°C, and 2.5 at. pct at 500°C. The phases Ta2C, the low-temperature modification of Ta205, and Ta,N of unknown composition but which has a superlattice structure based upon the original bcc tantalum lattice have been identified as the initial precipitates in the respective systems. Metallographic methods were employed to verify the X-ray analyses. The etching behavior of Ta is discussed in terms of lattice i?rzperfections and precipitate phases. The excellent fabricability, high melting point, and nuclear properties of tantalum are responsible for interest in this refractory metal. Data on the solid solubility of the interstitial elements (oxygen, nitrogen, and carbon) in tantalum and on the precipitate phases are somewhat limited. The significant contributions are discussed below. Because the purity of electron-beam melted tantalum (only recently available) is considerably higher than that used in previous studies, the present investigation was initiated. Gebhardt et all-3 have investigated the tantalum-oxygen and tantalum-nitrogen systems with particular reference to the changes in physical properties and to the rates of reaction between these gases and the metal. The solubility of oxygen in tantalum was reported2 to be 3.7 at. pet at 1500°, 2.3 at. pet at 100O°C, and 1.4 at. pct at 750°C. Schonberg4 reported that several oxide phases (Ta40, Ta,O, TaO and Ta,05) exist while X-ray studies by Gebhardtl showed only two oxides, Ta,05 and an unidentified phase which was associated with a platelet-type precipitate. La-gergren and Magneli,' however, questioned the existence of compounds other than the two allotropic modifications of Ta,05 for the tantalum-oxygen system. In the case of nitrogen, the solubility was estab- lished by Gebhardt3 to be of the order of 7 at. pct at 1800°c. The solubility was reported to decrease rapidly with temperature, and, although no limits were established, a precipitate phase was observed by Gebhardt except when the high-nitrogen specimens were cooled very rapidly from the reaction temperature of 1800c. He reported the initial precipitate phase to be a tetragonal distortion of the bcc tantalum lattice while Schonberg6 reported the phase lowest in nitrogen Jo be a cubic super-lattice with a cell size of 10.11 A. Two other nitride phases, Ta,N and TaN, were reported; these appear to be isomor-phous with the carbides of tantalum. The tantalum-carbon system was investigated by Ellinger7 and by Lesser and Braurer. Two compounds, Ta,C and TaC, were reported to exist, each with a range of composition. The solubility of carbon in tantalum was found to be practically nil at all temperatures. Thus, of the interstitial elements which are present in small amounts in high-purity tantalum, carbon might be expected to form precipitates. The present investigation was initiated to obtain additional data on the solid-solubility limits of these interstitials at 1500°, 1000°, and 500' with particular emphasis on the distribution and the identification of the precipitate phases. EXPERIMENTAL WORK AND RESULTS In the present investigations of the solid solubility and of the precipitate phases in the systems tantalum-nitrogen, -oxygen, and -carbon, high-purity tantalum was reacted with high-purity gases, homogenized at 1800°c, and annealed at and quenched from 1500°, 1000,

Jan 1, 1962

By Margaret V. Doyle, R. W. Powers

INTERNAL friction measurements, carried out as functions of temperature, have been used extensively to obtain data on the mobility of interstitial impurities in the Group V metals, vanadium, colum-bium, and tantalum. For a given frequency of vibration, the internal friction peaks at a temperature which depends principally on the particular metal and interstitial impurity. Relaxation times and corresponding activation energies are determined from a knowledge of such peak temperatures for various vibration frequencies. These experimentally determined relaxation times are related to the average jump frequencies of the interstitial impurity atoms using the model of Snoek1 and can be related to macroscopic diffusion coefficients as shown by Polder.2 In these Group V elements, the impurity whose diffusion rate has been the hardest to pin down by the internal friction technique has been carbon. The experimental difficulties associated with carbon in these metals were not evident in the earliest investigation carried out by Ke on tantalum.3 The carbon peak was thought to occur near 140°C at 1 cps on the basis of the enhancement of the height of this peak measured on specimens which had been coated with colloidal carbon and heated in vacuo at 1200°C. Presumably on the basis of similar evidence, Wert identified a peak also near 140°C at 1 cps in columbium with the diffusion of carbon in that element." Later, the difficulties of admitting carbon into these metals without simultaneously introducing oxygen were pointed out by Ang and Wert- nd by Marx, Baker, and Sivertsen.6 The latter suggested that the peaks attributed to carbon in tantalum and columbium might arise from the presence of traces of oxygen, adventitiously absorbed during the carburization. Such suspicion was confirmed, at least in tantalum, when it was found possible to prepare C-Ta specimens without contamination by oxygen. Specimens sci prepared, aitnough high in carbon content, gave no evidence of a damping peak near 140°C.7 Recently, the authors were able to Show that carbon diffuses in tantalum at a rate only slightly slower than that for nitrogen.8 At 1 cps, the carbon peak lies at 34g °C, only a few degrees above the nitrogen peak at 341 °C. However, the two could be distinguished by a different stability with respect to aging at 400 °C and by a different dependence of peak height on solute concentration. On the basis of this experience with tantalum, it appeared worthwhile to search also for a carbon peak in columbium in the vicinity of the nitrogen peak." In this report, the location of the carbon peak in columbium is made known and its position relative to the nitrogen peak is compared with the authors' previous findings in tantalum. In addition, a second source of internal friction seen only in specimens of very high purity is discussed. Columbium was obtained from the Fansteel Metallurgical Corp. as either 30 or 40 mil diam stock. The manufacturer gives the following analysis as typical of this material: 99.4 pct minimum Cb, 0.10 pct maximum C, 0.5 pct Ta, 0.04 pct Ti, 0.02 pct maximum Si, and 0.01 pct maximum Fe. Wires 13 in. long were degassed near 2200°C for 4 to 16 hr in an ultimate vacuum better than 2.10" mm Hg in an apparatus described previously.8 This treatment reduced the oxygen and nitrogen damping peaks observed in the as-received material to less than 0.0001 in Q-1 above background. The latter value varied somewhat from specimen to specimen in the range 0.0004 to 0.0008, depending chiefly on the wire diameter and the frequency of vibration. The high temperature evacuation left the specimen in a rather soft condition, the Vhn being reduced to 40 from a value near 121 in the as-received conGi~iur~. The gram size was about the diameter of the specimen. After outgassing, specimens were loaded with carbon by absorption of such hydracarbons as methane or ethylene. Carbon was also added to a few speclrnens by heating them at

Jan 1, 1958

By C. H. White

Discussion of a Paper by Mr. C. H. White, read at the Atlantic City Meeting, February, 1904. (Annual Meeting, February, 1005.) ARTHUR JARMAN, Sydney, New South Wales, Australia (communication to the Secretary*) : All designs for modern metal¬lurgical and chemical laboratories should provide each student's desk with a hood or cupboard for the removal of fumes, but I doubt the advisability of placing air-baths and similar apparatus close to the hot plate. It seems to me that unless the draft be exceptionally strong the fumes from ordinary wet assay work will corrode the iron-work of the fittings, in which case the baths would have to be removed to a general desk in order to lighten the work of the laboratory attendant. Since the laboratory described by Mr. White has been in use for two years, I should like to ask if any inconvenience has resulted from this corrosion. If not, it is certainly an important improvement to have the air-baths and similar apparatus placed -on the student's desk. The hoods described by Mr. White are supplied with a good draft by means of a fan, which gives them a great advantage over those at the metallurgical laboratory at the University, Sydney, in that no doors to the hood are needed. Each hood in the laboratory at Sydney is connected by a glazed earthenware drain-pipe with a vertical flue, 20 ft. high, having a lighted gas jet at the bottom to assist the draft. Although the draft is good, fumes of sulphuric acid cannot be drawn o$ unless the doors of the hood are lowered more than half-way. In my opinion, a fan should be used for the purpose of creating the draft, and glazed drain-tile should invariably be used for the flues because no other material possesses the same advantages. I know of a recent instance in which a laboratory containing

Mar 1, 1905

By Joseph E. Pogue

NEW economic forces are at work in the petroleum industry.. In order to visualize these forces and clearly see their bearing on the producer, refiner and marketer, it is necessary to see in perspective the economic evolution of the business. For several decades prior to 1913 the outstanding feature of the petroleum industry was a trend toward integration, culminating in a huge combine, the Standard Oil Co. An important aspect of this integrative trend, however, was its concentration on the combination aid control of refining and marketing, leaving crude oil production, for the most part, to the exigencies. of small-unit competition. It is a noteworthy coincidence that during this era the law of oil and gas was formulated and applied, whereby these substances had to be reduced to possession to establish ownership; and the forces of competition in crude oil production were thereby intensified. It was to the interest of an industry, safeguarded in its control of manufacturing and markets, to have supply stimulated by legal convention as well as by individual initiative in order that the growing demand could be met without interruption. And so over-production of crude oil during this era was no handicap, but rather an aid, to the progress of the industry.

Jan 1, 1929

By W. H. Blauvelt

THE subject of fuel-briquetting has attracted much attention on the part of engineers and investors for the past 15 or 20 years, and especially in recent years, during which a number of plants have been built, with more or less commercial and technical success. Our technical literature contains numerous descriptions of certain processes, and discussions of the industry in general. For a history of the development of the art in the United States, and for descriptions of many of the processes which have been tried, reference may be made to the files of our Transactions, and, for more recent information, to a paper by C. T. Malcolmson, read before the First Annual Convention of the International Railway Fuel Association in June, 1909. The purpose of the present paper is to describe the briquette-plant of the Solvay Process Co. and the Semet-Solvay Co. at Detroit, Mich., which, after a period of long and costly evolution, is now operating satisfactorily on a commercial basis. I believe that it will be of interest to some of our members to have the details of operation, lower-consumption, labor, etc., as worked out on a practical and commercial scale in a going operation. The briquette industry has had a somewhat checkered career in the United States, and much the larger portion of the failures has been due entirely to commercial causes. It seems axiomatic to say that before undertaking the installation of a plant for manufacturing briquettes it is necessary that the local situation should be carefully examined : First, to determine the kind of briquettes, if any, the local market will consume; that is-to say, whether the available fuel-supply is such that briquettes would be a welcome addition, and whether the most promising field is the industrial or the domestic market. Second, if there is an available supply of raw material, as coal,

Mar 1, 1910

By A. R. Troiano, E. A. Steigerwald, F. W. Schaller

D. N. Williams(BatteZle Memorial Institute)-The authors have presented an extensive collection of arguments pertaining to the role of stress in hydrogen embrittlement. The basic assumption of these arguments is that stress is essential as a driving force for diffusion of hydrogen. However, in view of the rapid diffusion rate of hydrogen in steel at low temperatures as evidenced by the ability to alloy with hydrogen by electrolytic charging, it seems unlikely to me that stress acts in this manner. Instead, I would like to suggest that stress may be essential for the nucleation of hydrogen in steel. I believe that such an assumption would equally well satisfy the experimental data presented by the authors. I should also like to comment on the interpretation of the data presented in Figs. 5 and 6. Fig. 5 shows the effect of hydrogen content on ductility in a rupture test. The curve as drawn by the authors indicates an abrupt transition from ductile to brittle behavior at about 0.001 amp per sq in. (5 ppm). The data points would equally well support a gradual transition from ductile to brittle behavior extending over the range from 0.0008 to 0.02 amp per sq in. (4 to 8 ppm). A gradual transition would be the ex-

Jan 1, 1962

By Mara Kosovac, Sujan K. Kundu

The Iron Ore Co. of Canada (IOC) has developed a computerized plan analysis method for its open-pit iron mining operations which will eliminate much of the tedious manual drafting of pit design plans performed by engineers and geologists at its two major operational areas near Schefferville, Que., and Labrador City, Nfld. The new technique permits analysis of section or bench plans for a specific ore body, based on drillhole information; preparation of a three-dimensional unit profit matrix for pit design purposes, and storage of extensive ore-block information for other applications. Other advantages include enhanced design accuracy through reduction of human errors normally associated with preparation of large data masses, and by elimination of errors inherent in planimeter-prepared ore block diagrams.

Jan 7, 1978

By JOHN D. SUMMER

THE Premium Price Plan for copper, lead, and represent, the approach of the Office of Price Administration to the urgent of wartime problem of securing increased output of nonferrous metals. Some of the problems encountered in too operation of the Plan and the considerations which led to it?s adopt it will here he reviewed. The Plan provides for extra payment by the Metals Reserve Co., to mine operators who exceed established quotas of production. Producers are thus directly, compensated for the higher costs of working ores that are not commercial at the ceiling price, although the metal obtained from these ores is directed into regular channels of distribution at the established prices for copper, lead, and zinc. Higher-cost metal is thus available to fabricators and to the government agencies at the regular ceiling price and the dual objective of increased production and table pries is achieved.

Jan 1, 1943

By D. Van Winkle, C. Zener, H. Nielsen

THe internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. Experimental Method The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress, The general method of making such measurements, and of observing temperature of a specimen during a measurement, has been described.5.6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and goo cycles per second. Specimens The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alpha-brass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at .successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n1/2 where n is the mean number of grains per square millimeter. Experimental Results This paper is concerned exclusively with the part of the internal friction that be. comes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

By C. Zener, H. Nielsen, D. Van Winkle

THe internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. Experimental Method The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress, The general method of making such measurements, and of observing temperature of a specimen during a measurement, has been described.5.6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and goo cycles per second. Specimens The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alpha-brass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at .successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n1/2 where n is the mean number of grains per square millimeter. Experimental Results This paper is concerned exclusively with the part of the internal friction that be. comes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

By W. D. Faulkner, J. E. Urbanic, R. J. Jula

The process of treating granular activated carbon for return to service in the recovery of gold in carbon-in-pulp and carbon-in-leach circuits has been investigated. Carbons from two US mines, one Canadian mine, and a South African pilot plant operation were characterized before and after regeneration. Thermal regeneration of the carbon was investigated using factorial analysis to determine the effect of interaction of furnace temperature, retention time, and use of supplemental steam. The operation of acid washing the service carbon was investigated, including a comparison of the use of nitric and hydrochloric acids. The effect of quenching regenerated carbon was also briefly studied. Prom the data obtained, guidelines are given for effective regeneration operation.

Jan 1, 1986

By Clarence Zener

The internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites, localized weak regions introduced by cold-working,6'7 grain boundaries and possibly twinning planes.8'9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, 3.i in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff. Experimental Method The experimental method used has previously been described in institute papers.5'6'9 The measure of internal friction adopted here, I/Q, is X the logarithmic decre- ment, a measure used by some writers, and is also X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the fundamental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. Experimental Results The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°C. As shown in Fig. I, the internal friction increased by only a factor of 2 from room temperature to 300°C., then by a factor of 100 during the next Ioo° interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction e-H/RT [I]

Jan 1, 1943

By Clarence Zener

The internal friction of nonferrous metals vibrating at low stress amplitudes has so far always been successfully interpreted in terms of inhomogeneities of one sort or another. Examples are the fluctuation of stress across a specimen vibrating transversely,1,2,3 the stress inhomogeneities due to the elastic anisotropy and partial random orientation of the individual crystallites, localized weak regions introduced by cold-working,6'7 grain boundaries and possibly twinning planes.8'9 Perfect single crystals are, by definition, homogeneous. Actual single crystals usually, perhaps always, contains some imperfections. The present investigation was undertaken to determine whether the internal friction of single crystals may likewise be attributed to inhomogeneities. This study was made possible through the gift of a large single crystal of 70-30 alpha brass by H. L. Burghoff, of the Chase Brass and Copper Co. The specimen, 3.i in. in diameter and 10 in. long, was similar to samples previously described by Mr. Burghoff. Experimental Method The experimental method used has previously been described in institute papers.5'6'9 The measure of internal friction adopted here, I/Q, is X the logarithmic decre- ment, a measure used by some writers, and is also X the specific damping capacity, a measure used by other writers. In all measurements the stress level was kept so low that the measurements were independent of stress level. In all measurements in which the temperature was varied, observations were made as the specimen slowly cooled from its highest temperature. The specimen was vibrated transversely. Observations were made at the fundamental frequency and at the first overtone, of about 620 and 1710 cycles per second, respectively. No attempt was made to avoid acoustical losses. Experimental Results The specimen was annealed for several hours at 450°C. The temperature dependence of the internal friction was then determined from room temperature to 400°C. As shown in Fig. I, the internal friction increased by only a factor of 2 from room temperature to 300°C., then by a factor of 100 during the next Ioo° interval. These measurements are consistent with the view that the observed internal friction is the superposition of two distinct parts. One, dominant at room temperature, is nearly independent of temperature. This part may be accounted for by acoustical losses and by transverse thermal currents. It was not further investigated. The second part, when plotted in the manner of Fig. I, lies upon a straight line. Therefore it has a heat of activation H; i.e., it varies with temperature as Internal friction e-H/RT [I]

Jan 1, 1943

By Thomas T., Read

TWO American students entered the Ecole des Mines in 1856, Joseph Lesley of Philadelphia and Thomas Egleston of New York. Lesley remained there only one year, but Egleston completed the whole 'curriculum and received, in 1860, the certificate given to foreign students .in lieu of the official appointment and degree. awarded French students. Returning home he received, in 1861, an appointment by Secretary Henry of the Smithsonian Institution to sort, label, and arrange the collections of mineralogical and geological specimens which had been brought to Washington by the various government exploring expeditions in the West. Thomas Egleston, born in New York City on Dec. 9, 1832, was the son of Thomas Jefferson Egleston, who came to New York from Massachusetts some time before 1829. The first American ancestor of the family had settled near Dorchester. in 1630. T. J. Egleston and Joseph Battell established an iron-merchandizing business* at 166 South St., New, York, which prospered exceedingly; so much so that when Thomas J. Egleston died, July 12, 1861, his estate had a book value of over $500,000. Since an older brother was expected eventually to take over this business, Thomas, who had a liking for science, went to Yale,, where he completed the regular four-year course in 1854, and then remained another year for advanced work in chemistry under Silliman. I One biographer says he went to Europe, . early in 1-856, on account of his health. It was the custom at that time for wealthy young men to make a tour of Europe after completing their academic education. Whatever the precise reason, he began scientific work at the Jardin des Plantes in Paris but soon trans* It still operating as Egleston Bros. Inc., though no direct descendants of its founder are now living.

Jan 1, 1941

By AIME AIME

NO MORE SUITABLE time and place than LOS Angeles on Thursday and Friday, July 28 and 29, could have been chosen for the Western Regional Meeting of the~1nstitutk. After attending two clays of technical sessions and enjoying the luncheons and dinners of the meeting, visitors, on the following days, could see the opening ceremonies and events of the Olympic Games, which started on July 30 and continued to Aug. 14. Such d spectacle can be seen only once in a generation in this country.

Jan 1, 1932

By C. Zener, H. Nielsen, D. Van Winkle

THE internal friction of metals has been studied frequently at elevated temperatures.1-4 In most cases it rises rapidly with increasing temperature. The notable exceptions are ferromagnetic materials, and lead.2 This paper describes an investigation of the general features of the high-temperature internal friction of 70-30 alpha brass. EXPERIMENTAL METHOD The internal friction of a metal is a measure of the rate at which it dissipates energy of vibration. The measure adopted here, I/Q, is (I/2p) times the specific damping capacity, a measure commonly used by engineers. In the measurements of this investigation, the stress level was kept so low that the observations were independent of the stress. The general method of making such measurements, and of observing the temperature of the specimen during a measurement, has been described elsewhere.5,6 The driver and detector coils were wound with wire insulated with glass thread, in order to withstand the high temperatures used. In previous work electrical eddy currents in the specimen served as the coupling between the mechanical vibration of the specimen and the electrical circuits of the driver and detector. The high values of the internal friction in the present investigation rendered this coupling insufficient. In order to increase this coupling, pole pieces cut from ordinary telephone diaphragms were attached to the specimen. A mixture of French chalk and water glass proved a satisfactory cement. All measurements were made at the fundamental frequency for transverse vibration, which lay between 600 and 900 cycles per second. SPECIMENS The measurements described herein were made upon a single cylindrical rod of brass, kindly furnished by Dr. Cyril Stanley Smith, of the American Brass Co. This rod was the specimen E of the set of alphabrass rods described in an earlier paper.6 Successively larger grain sizes were obtained by annealing at successively higher temperatures. A slice was cut off one end after each set of measurements. Grain counts were made on each slice by W. E. Lindlief, of the American Brass Co. Nine fields were viewed on each piece, located as shown in Fig. I. Results are given in Table I. The grain size is defined in the usual way; namely, Grain size = I/n ½ where n is the mean number of grains per square millimeter. EXPERIMENTAL RESULTS This paper is concerned exclusively with the part of the internal friction that becomes dominant at high temperatures. It is thus desirable to separate this part of the internal friction from the part that is

Jan 1, 1942

By J. A. Richardson

J. A. RICHARDSON[t]-Mr. Stuckey's account of the geology of the kaolins of North Carolina suggests that they exhibit some features similar to those of the Malay Peninsula. About one half of British Malaya (some 26,000 square miles) is occupied at the surface by igneous rocks, of which granite and its associated derivatives constitute fully 90 pct. The average granite is a biotic variety. It is predominantly potassic but carries, in addition, notable amounts of soda and lime so that albite and albiteoligoclase are generally common constituents of the rock. The minor derivatives from granite "magma" likewise include potassic and sodi-potassic members. Decomposition of the granitic rocks has led to the formation of kaolin in many localities, but, in general, the deposits are rather small and, at present, none is exploited commercially. True primary or residual kaolins (as defined by Stuckey; p. 48 Vol. 173, p. 2 TP 2219) have been developed from feldspar veins, pegmatites and from other granitic differentiates which cut through the larger masses of granite; they are usually small and narrow. Kaolin has been derived from aplite, quartz porphyry, quartz micro-porphyry, felsites and microgranites belonging to a complex known as the Chegar Perah-Pulai intrusion in northwest Pahang and southwest Kelantan. The bulk of the component rocks has been more or less strongly sheared. Kaolin-like end products have been formed from both sheared and nonsheared varieties. Kaolin has been formed also by the complete breakdown of trondjemite flanking the northwestern and western margins of the complex Bukit Ranjut syenite intrusion in northwest Pahang. These trondjemites range in composition from essentially quartz-free albiteplagioclasites to quartz-free microcline rocks; they are, in effect, the syenitic homologues of white sodic and potassic granite-aplites. The granites in Malaya have generally undergone more or less severe surficial weathering leading to the production of a spongy and rather cellular or a soft "mealy" material (sandy clay) down to depths of about 100 ft; in places the granite is strongly decomposed down to 150 ft. There has occurred, therefore, widespread partial kaolinization, but, in general, no extensive deposits of good quality kaolin seem to have been formed by these processes of decay. Frequently, the katamorphic processes of desilicification have advanced beyond the production of kaolin towards the formation of lateritic end products. The more important Malayan kaoiins seem to be confined to the western alluvial plains, particularly in areas either where granite crops out at surface, or where it forms the bedrock of the alluvium. There are numerous excellent examples around Gopeng and elsewhere in the Kinta Valley of Perak. Such kaolins belong to Stuckey's groups of secondary deposits, and, like them, these also may be bedded. Field observations have established the existence of what for want of a better name is referred to by the Malayan Geological Survey as "granite wash." It is believed that granite, undergoing extensive deeply penetrative and probably rather rapid destruction under humid tropical weathering (temperature around 90°F; rainfall about 100 in. per annum; high humidity) "flowed," was moved by "creep" and, in addition, probably slumped in large waterlogged masses of sandy clay from topographic salients onto the adjacent flats. Either during this period of transmigration or later when the sludged granite detritus, after having more or less come to rest, was attacked by flowing water, differential sorting and erosion took place with the result that the resorted debris was moved and later deposited as bedded alluvium. In this way, banded "granite wash" was produced comprising alternating bands of clayey sand (resorted granite sludge) and white

Jan 1, 1947

By T. M. Morris

A SEARCH of the literature reveals that no measurements have been made of the forces acting between a small solid particle whose surface is hydrophobic, and an air bubble to which the solid adheres, both immersed in water. Analyses have been made of the forces acting to support a greased solid on the surface of water, and the forces acting to cause a solid, whose surface is hydrophobic, to adhere to an air bubble in water. The latter analysis T. M. MORRIS, Junior Member AIME, is in the Department of Metallurgical Engineering and Mineral Dressing, School of Mines and Metallurgy, Rolla, Mo. New York Meeting, February 1950. TP 2734 B. Discussion of this paper (2 copies) may be sent to Transactions AIME before Feb. 28, 1950. Manuscript received May 16, 1949. This paper is the result of work done for part of a doctor's thesis at the Missouri School of Mines and Metallurgy. is often incomplete, however, because the internal pressure of the bubble has been neglected. It will be demonstrated that the internal gas pressure is not a negligible factor when dealing with bubbles of the size encountered in flotation. A study of the forces acting between an air bubble attached to a large flat surface is informative. It must be borne in mind, however, that this is not the condition present in a flotation cell, where the particle is small compared to the size of the bubble. The bubble is allowed to spread to its maximum contact angle on a large flat surface in the first case, whereas in the second case, the spread of the bubble is limited to the surface of the small particle which is presented to the bubble. Kabanov and Frumkinl studied the forces acting to cause adhesion of bubbles of hydrogen to a large surface of mercury, which served as an electrode in a dilute sulphuric acid solution. The force acting to hold the bubble to the mercury surface was found to be the vertical component of the surface tension between hydrogen and the sulphuric acid solution. The forces tending to cause the bubble to separate from the mercury surface were found to be: (1) the force exerted due to the internal pressure of the bubble acting upon the area of contact between the bubble and the mercury surface, and (2) the buoyant force of the bubble minus the hydrostatic force acting at the base of the bubble. These investigators photographed bubbles that were just on the verge of separating from the mercury surface. From these photographs, they measured the contact angle between the mercury surface and the tangent to the hydrogen-solution interface at the point of contact between bubble and mercury surface. They calculated the volume of the bubble and the internal pressure of the bubble. The equivalence between the upward acting and downward acting forces was remarkable. Wark2 pursued an investigation similar to that of Kabanov and Frumkin, and at the same time. His deductions verified those of Kabanov and Frumkin. He also considered the conditions present in flotation and was aware of the effect of the internal pressure of the bubble. Further, he proposed several conditions under which a small solid particle would adhere to an air bubble in water. In 1922, Edser," an English physicist, made the following statement. "It must be remembered that no particle could float stably, but for the possibility of variation of the contact angle, for if this were a constant, a slight tilt would inevitably cause the particle to sink." Wark criticized this statement, maintaining that the contact angle does not vary. The experimental data to be presented indicates that Edser was correct. Experimental Procedure: Briefly, the experimental procedure was as follows. A bubble of air was generated in distilled water. A rod of known diameter, one end of which was water repellent, was attached to this bubble. The weight of the 'rod was measured. The internal pressure of the bubble was measured with a manometer. The hydrostatic head from the surface of the water to the bottom of the rod was measured. The angle between the horizontal projection of the end of the rod and the tangent to the bubble at the circle of contact be-

Jan 1, 1951

By T. M. Morris

A SEARCH of the literature reveals that no measurements have been made of the forces acting between a small solid particle whose surface is hydrophobic, and an air bubble to which the solid adheres, both immersed in water. Analyses have been made of the forces acting to support a greased solid on the surface of water, and the forces acting to cause a solid, whose surface is hydrophobic, to adhere to an air bubble in water. The latter analysis T. M. MORRIS, Junior Member AIME, is in the Department of Metallurgical Engineering and Mineral Dressing, School of Mines and Metallurgy, Rolla, Mo. New York Meeting, February 1950. TP 2734 B. Discussion of this paper (2 copies) may be sent to Transactions AIME before Feb. 28, 1950. Manuscript received May 16, 1949. This paper is the result of work done for part of a doctor's thesis at the Missouri School of Mines and Metallurgy. is often incomplete, however, because the internal pressure of the bubble has been neglected. It will be demonstrated that the internal gas pressure is not a negligible factor when dealing with bubbles of the size encountered in flotation. A study of the forces acting between an air bubble attached to a large flat surface is informative. It must be borne in mind, however, that this is not the condition present in a flotation cell, where the particle is small compared to the size of the bubble. The bubble is allowed to spread to its maximum contact angle on a large flat surface in the first case, whereas in the second case, the spread of the bubble is limited to the surface of the small particle which is presented to the bubble. Kabanov and Frumkinl studied the forces acting to cause adhesion of bubbles of hydrogen to a large surface of mercury, which served as an electrode in a dilute sulphuric acid solution. The force acting to hold the bubble to the mercury surface was found to be the vertical component of the surface tension between hydrogen and the sulphuric acid solution. The forces tending to cause the bubble to separate from the mercury surface were found to be: (1) the force exerted due to the internal pressure of the bubble acting upon the area of contact between the bubble and the mercury surface, and (2) the buoyant force of the bubble minus the hydrostatic force acting at the base of the bubble. These investigators photographed bubbles that were just on the verge of separating from the mercury surface. From these photographs, they measured the contact angle between the mercury surface and the tangent to the hydrogen-solution interface at the point of contact between bubble and mercury surface. They calculated the volume of the bubble and the internal pressure of the bubble. The equivalence between the upward acting and downward acting forces was remarkable. Wark2 pursued an investigation similar to that of Kabanov and Frumkin, and at the same time. His deductions verified those of Kabanov and Frumkin. He also considered the conditions present in flotation and was aware of the effect of the internal pressure of the bubble. Further, he proposed several conditions under which a small solid particle would adhere to an air bubble in water. In 1922, Edser," an English physicist, made the following statement. "It must be remembered that no particle could float stably, but for the possibility of variation of the contact angle, for if this were a constant, a slight tilt would inevitably cause the particle to sink." Wark criticized this statement, maintaining that the contact angle does not vary. The experimental data to be presented indicates that Edser was correct. Experimental Procedure: Briefly, the experimental procedure was as follows. A bubble of air was generated in distilled water. A rod of known diameter, one end of which was water repellent, was attached to this bubble. The weight of the 'rod was measured. The internal pressure of the bubble was measured with a manometer. The hydrostatic head from the surface of the water to the bottom of the rod was measured. The angle between the horizontal projection of the end of the rod and the tangent to the bubble at the circle of contact be-

Jan 1, 1951

By J. P. Zannaras

If we assume that testing of the model started at time t1, that time t2 was the instant at which the elastic limit of the material was passed at the points of the maximum stress, and that at time t3 the failure of the model was completed as shown in the typical photograph (Fig. I), then actually the photograph shows the final results of what took place between time t2 and t3. By the principle of similitude all conclusions drawn from the behavior of the model were applicable and valid for actual mine roofs up to the time t2 after time t2 motions and friction came into play during the destruction of the model. The events between t2 and t3 and the photograph itself are not representative of the events expected in an actual mine roof unless corrections imposed by the principle of similitude are made. It can therefore be stated that all conclusions and observations of the author from the photographs are applicable only to his small-scale experiments and not to actual mine roofs. Without investigation of the true stresses or the combined maximum stress induced in the beds it has been assumed by the author that failure occurred solely due to bending stress caused by loading of the beds. (The author states that D was taken to be the theoretical strain given by elementary beam theory.) Fig. 1 shows that the beds were clamped together. This clamping was necessary to prevent slipping of the beds due to the horizontal shear. However, this clamping caused an uncontrolled and undertermined com-pressive stress S at the end of the beds, and this com-pressive stress caused a true tensile stress ?S (? PoiS-son ratio). This true tensile stress combined with the tensile stress produced at the end of the beds due to loading (fixed beam uniformly loaded), and the horizontal shear which is maximum at the end appears to be the most probable maximum stress produced in the beds. It is therefore evident that the author in performing this experiment has introduced stresses in the model not existing or dissimilar to actual mine roofs, and therefore his conclusions may be applicable to his small-scale experiments but inapplicable to actual mine roofs. Louis A. Panek (author's reply)—The discusser's difficulty is related to mechanics of materials rather than similitude. The effect of time did not enter into the tests in any way, being simply excluded from consideration in this study, because all quantitative results entering into the design equations are based on measured (between time t1 and time t2) bending strains that are well below the breaking strain (i.e., in the elastic range) for the model material. Time does not become a significant factor until the rock stress reaches 80 to 90 pct of the breaking stress." The objective of this investigation was not to predict that bolted roof will fail after time t, but was instead to develop a safe roof, that is, roof in which the bending strain is much less than (say less than 50 pct of) the breaking strain. The models tested to failure had no direct bearing on the design equations. Although for some rocks time may influence the magnitude of stress or strain at which fracture occurs, breaking stress or breaking strain values were not employed for any purpose in this investigation. Tests to failure were made only to obtain additional evidence regarding the behavior of the bolted laminae' as evinced by the locations of the cracks. As stated in the last paragraph of the paper, if one wishes to predict the time or stress conditions for which the roof will fail, additional information is required. The reason for clamping the laminae is to make them behave liked clamped beams, which closely approximate the clamped-plate condition of the actual mine roof beds (Ref. 5, p. 1; Ref. 6). The writer has previously demonstrated that the bending stresses induced by centrifugal loading in a clamped model beam are in agreement with those predicted by theory;' hence clamping has no significant effect on the bending ,trains measured during a test. Moreover, actual ,in, roof beds are likewise subject to a clamping effect due to weight of superincumbent strata carried by the pillars or ribs on each side of the opening. It is emphasized that this study was restricted to evaluating only the reinforcing effect produced by the bolts. Procedures employed in the experiments and in the data analysis were such as to deliberately exclude the effects of other factors. The objections offered are therefore invalid,

Jan 1, 1957