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By A. G. H. Andersen, A. W. Kingsbury

SILICON bronzes containing iron are used to a considerable extent in industry, under the trade name of P.M.G. alloys. Various classes of wrought alloys fall in the composition range 1.5 to 3.5 per cent silicon, and 0.5 to 2.5 per cent iron. Castings may contain as much as 6 per cent silicon and 3 per cent iron at present. The constitutional diagrams of these alloys are thus of considerable practical importance. Copper-silicon-binary alloys have been thoroughly investigated by a number of workers, the latest reports being those of C. S. Smith1 and of A. G. H. Andersen.2 Although much work has been done on iron-copper alloys,3 recorded investigations on the copper-rich copper-iron binary constitutional diagram are not numerous. Tammann and Oelsen4 determined the solubility limits of iron in copper by means of magnetic measurements, and found that the solubility of iron in copper amounts to a fraction of one per cent at 400°C., increasing slowly to one per cent at 800°C. From 800°C., the solubility increases rapidly and attains 4 per cent at 1100°C. Hanson and Ford,5 using electrical resistivity measurements and the microscope, determined a somewhat different solubility limit. Of earlier X-ray works on the copper-iron system, very little has been published. The work by Bradley and Goldschmidt6 on copper-iron-aluminum alloys includes some information on the copper-iron binary. These investigators conclude that substitution of iron in the copper lattice decreases the spacings, which is contrary to the evidence of the present work. Hanson and West7 have investigated the ternary alloys of copper with iron and silicon. Although their diagrams are valuable contributions to the understanding of these alloys, they did not recognize the kappa phase,12, 7,8 and their diagrams do not everywhere conform to the phase rule. The present work contains a check by means of X-rays of the solid solubility limit of iron in copper, and an X-ray investigation of the ternary-phase diagram, which, owing to present conditions, it became necessary to curtail considerably. PREPARATION OF SAMPLES Castings weighing about 75 grams were melted under vacuum. The charges were made up of ingot iron, copper cathodes from Laurel Hill, and refined silicon supplied by the Electrometallurgical Co. Alundum crucibles were generally used. The exceptions were alloys 77 and 78, which were melted in graphite crucibles. The ingots were annealed at 800°C. for one week, then samples were cut for chemical analysis. Longitudinal sections of the binary alloy ingots were hammered into plates 3 in. thick. Wherever possible, these plates were homogenized at temperatures ensuring

Jan 1, 1942

By Albert Ladd Colby

PAGE I. Introduction,...........577 11. PRocess of Manufacture. 1. American Specifications. 2. Foreign Specifications, . ......... 580 III. Chemical Properties. I. Chemical Composition: (a) American Specifications ; (b) Foreign Specifications. 2. Chemical Analysis: (a) American Specifications ; (b) Foreign Specifications ; (c) Number of Analyses Required ; (d) Sample for Analysis ; (e) Check-Analyses Impracticable ; (f) Rejection Solely on Variation in Com-' position,............581 IV. Physical Properties. 1. Drop-Test and Drop-Testing Hachine: (a) American Specifications ; (b) Foreign Specifications ; (c) Limits in Deflection. 2. Tensile Test: (a) American Specifications; (b) Foreign Specifications ; (c) Test-Pieces are not Representative ; (d) Specified Tensile Strength is Affected by the Section ; (e) BpeciBed Tensile Strength is Often Inconsistent with Specified Chemistry ; (f) Specified Tensile Strength is Often Inconsistent with Specified Elongation ; (g) Amount of Tensile Testing Required is Excessive ; (11) Conclusions. 3. Dead-Weight Test: (a) American Specifications; (b) Foreign Specifications; (c) Number of Tests Specified. 4. Bending-Test: ((1) American Specifications ; (b) Foreign Specifications,..........589 V. Section. 1. American Specifications. 2. Foreign Specifications: (a) Templets ; (b) Sample Piece of Rail; (c) Allowable Variation from Templet,...........601 VI. Weight. 1. American Specifications. 2. Foreign Specifications,. . 603 VII. Length. 1. American Specifications. 2. Foreign Specifications, . . 604 VIII. Drilling. 1. American Specifications. 2. Foreign Specifications, . 604 IX. Finish. 1. American Specifications. 2. Foreign Specifications, . . 50.5 X. Branding. 1. American Specifications. 2. Foreign Specifications : (a) Data to be Rolled in Raised Letters on Web of Rail ; (b) Marking of the Blow-Number on Each Rail; (c) Additional Marking and Painting of Rails,........605 XI. Inspection. 1. American Specifications. 2. Foreign Specifications: (a) Prior Notice of Rolling; (b) Free Access to the Works ; (c) Cost of Inspection, Analyses and Tests to be Borne by the Manufacturer ; (d) Rails after Inspection by Manufacturer to be Sorted into Lots Prior to Inspection by the Engineer ; (e) Disposition of Rejected

Jan 1, 1907

By D. E. Stephenson. Discussion by R. G. K. Morrison, L. Obert

R. G. K. Morrison (Chairman, Dept. of Mining Engineering and Applied Geophysics, McGill University, Montreal, Que., Canada) - The discing of drill core has been a recognized pressure phenomenon for many years but only recently has an interest been taken in the mechanism involved. The work of Jaeger and Cook is referred to in the text. The authors have now advanced the study to establish, within certain loading limitations, a direct relationship between axial and radial stress at failure. This is an important contribution. In mines generally, where pressure conditions result in the spalling of openings, the faces of drifts and crosscuts, on scaling, usually show a concavity with respect to the opening very similar to the face of the drill hole after the separation of the stub. The same holds for shaft sinks. This suggests a similarity between the mechanism of the discing of core and that of the spalling of an opening, under pressure, to develop a more stable outline. The latter, commonly regarded as shear, is the most conspicuous type of failure observed in

Jan 1, 1967

By W. F. Hosford

W. F. Hosford, (Massachusetts Institute of Technology) —evelopment of methods for predicting the plastic anisotropy of textured metals is an important step toward the improvement of properties by texture control. The engineering value of the present analysis is indicated by the good agreement between prediction and experimental findings. The purpose of this discussion, however, is to point out the weakness of the assumptions on which the analysis is based. The authors state that "the relative width and thickness strains are believed to depend only on the slip direction" and accordingly they disregard the orientation of the active slip plane. where E,, cW, and et are the tensile, width, and thickness strains, A,, A,, and At are the angles between the tensile axis x, the width direction w, and the thickness direction t, respectively; and G,, GW, and 4 are the angles between the slip-plane normal and x, w, and t, respectively. Therefore, the ratio of width to thickness strains resulting from slip on a single system would be These relations hold regardless of whether the slip plane is a crystallographic plane of the {110}, (1121, or (123) type or whether noncrystallographic slip occurs. If noncrystallographic slip occurs, it might be reasonable to assume that the effective slip plane is the most highly stressed plane containing the slip direction. In this case the slip direction, S.D., the slip plane normal, S.P.N., and the tensile axis, x, are coplanar (Fig. 19) and the angles are related by following expressions: where 9 is the angle between t and the projection of the slip direction in the w-t plane (igs. 1 and 2). The normal strains, Eq. [9], become

Jan 1, 1963

By W. A. Backofen

THE texture of cold-drawn copper wire has been described most often as a composite of [Ill] and [loo] directions aligned parallel to the wire axis.' Hibbard2 suggested that sufficient reduction will result in a single [111] texture and reported that after a reduction in area of 96.4 pct, such a texture was nearly obtained. Other work3-4 has shown that recrystallization within the temperature range of 300" to 1000°C does not alter the texture established by cold-drawing. In general, however, the texture of cold-drawn end annealed copper wire is not as well defined as the deformation texture. In the work reported here it was found that the double-fiber, deformation texture persists even after a reduction in area of 97.3 pct, and after recrystallization the texture is practically all [l00]. The wire used in this work was prepared in the following way. A 3/4-in. diam length of annealed OFHC copper was cold-drawn to a diameter of 1/8 in., a reduction in area of 97.3 pct. Each step in the drawing operation brought about a reduction in area that varied from 6 to 10 pct. Short lengths of this wire were etched in a 50-pct solution of nitric acid to a diameter of approximately 0.01 in. The texture of the cold-drawn specimens was determined with the conventional X-ray transmission diffraction technique using filtered copper radiation. The X-ray beam was directed perpendicularly to the wire axis and the diffraction rings were recorded on a flat film. Fig. la is typical of the photo-grams obtained and reveals that the cold-drawing schedule described above introduces a distinct, double-fiber texture with both [Ill] and [l00] directions aligned parallel to the wire axis. Supplementary measurements with a Geiger-Mueller counter of the intensity of reflection from (111) planes showed that the [111] component was much more predominant than the [l00]. Additional specimens of the drawn and etched wire were annealed in a salt bath at temperatures from 300" to 450°C. The texture of the recrystal-lized wire was studied with the same technique applied to the cold-drawn wire. Fig. lb is an X-ray photogram of a specimen annealed for 1 ½ at 300°C and is typical of those obtained from re-crystallized specimens. The photogram shows that recrystallization of this material is accompanied by the almost complete elimination of the [111] component of the deformation texture. A pronounced strengthening of the [100] component was evident from intensity measurements with a Geiger-Mueller counter. In summary, the deformation texture of cold-drawn OFHC copper wire, after a reduction in area of 97.3 pct, may still be described as a composite of [Ill] and [loo] directions aligned parallel to the wire axis. Recrystallization of such wire at temperatures from 300" to 450°C introduces a texture which consists almost entirely of a [loo] alignment. Acknowledgment Sidney Rolle of the Scomet Engineering Co. generously supplied the OFHC copper used in this work. References 'C. S. Barrett: Structure of Metals. p. 382 (1943) New York. McGraw-Hill Book Co. 2 W. R. Hibbard, Jr.: Trans. AIME (1949) -185, p. 598; Journal of Metals (Sept. 1949) TN 19E. 3 P. 422 of ref. 1. 'E. Schmid and G. Wasserman: Ztsch. Physik (1926) 40, p. 451.

Jan 1, 1952

By AIME AIME

READERS of a technical paper, or the audience if the paper is presented orally, judge the paper on several counts. The September 1940 issue of MINING AND METALLURGY contained an excellent short article by S. Marion Tucker en- titled "Are You Going to Present a Paper," which considered the general subject of presentation. In it Dr. Tucker referred to the large number of poorly prepared and badly delivered papers that are presented annually before the large number of technical and other societies that meet regularly, and he stressed the point that good delivery, length of paper, content, and composition are of great importance. All of Dr. Tucker's points were well taken; however, good illustrations are equally important in explaining certain phases of some papers.

Jan 1, 1941

Book Review MANAGEMENT AND MEN. By Meyer Bloomfield, Boston. The Century Co., New York, 1919, pp. 584, H.X. 5 1/2. $3.50. This hook is an exposition of English efforts to solve the problem of labor unrest in England. The first six chapters are reprinted from articles published in the Satur-day Evening Post, for whom the author went to England to study the problem at first hand. These articles deal with housing, increased production, eliminating the internal friction in the industrial machine and a chapter each devoted to the view-point of employer and employee. These chapters are written in the easily readable magazine style and give a complete general survey of the particular solution being tried. Perhaps their greatest., certainly not their least, worth lies in the fact that they form a vehicle for unusually voluminous appendices containing in full the famous Whitley Reports which are the basis of the new movement, together with various reports, which, except for this publication, would be largely inaccessible to those inter-ested in this country. The Whitley scheme considers each industry a unit and proposes to establish therein a Joint Standing Industrial Council composed of representatives of employers and employees to consider appropriate matters affecting the industry at large. There is to be a District Council for each industry which will, as its name implies, deal with the clatters pertaining to that interest in. the particular district. The third and last body in this scheme of Industrial Parliament is the Works Committee, which is com-posed of representatives of the management and of the workers employed in particu-lar plants or mines to act in close cooperation With the district quid national machinery. The Whitley or similar schemes have been tried in many communities in England and the book contains interesting comments on the result obtained, it being notable that most of the objections conic from plants which have not tried the scheme. Meyer Bloomfield, the author; is the specialist in industrial personnel problems who organized the industrial service activities of the United States Shipping Board, Emergency Fleet Corporation. P. E. B.

Jan 10, 1919

The program of 'the Chicago meeting, which is to be held Sept. 22-26, is as follows: Monday. Morning-Registration. Afternoon-Technical Session. Evening Smoker. Tuesday. Morning and Afternoon-Excursion by boat to Gary and trip, through United States Steel Co's. plant. Evening-Technical Session. Wednesday. Morning- Technical Session. Afternoon-Technical Session. Evening-Banquet, Congress Hotel. Thursday. Morning and Afternoon-Special train to La Salle and De Pue, Ill., Inspection of Zinc Smelters, Cement Works, and Coal Mines. Trip to Starved Rock and points of historical interest. Evening-Return by train to Chicago. Friday. Morning-Optional trips. 1. East Chicago Metallurgical Plants and Oil Refineries at Whiting, Ind. 2. North Chicago and Milwaukee. 3. Local Chicago Plants. 4. Coal trip to Franklin and McCoupin Counties.

Jan 6, 1919

By S. W. MEALS

TWENTY million people in this country and Canada in nearly four million homes can give thanks to our Creator for natural gas, that most wonderful natural fuel with which Dame Nature has so bountifully blessed us. It is a clean, healthy and cheerful fuel, made up almost entirely of carbon and hydrogen. There is no residue, no waste and there are no objectionable constituents; an ideal fuel for the home. It operates like magic, open the valve and it is there for your needs, winter or summer, night or day. You are not required to place your order 30 to 90 days in advance and you do not need to pay for your winter's supply in advance. No ashes to worry about, no flues or chimneys to clean, nor kindling wood to store or bother the housekeeper. We who have been so blessed do not realize what it would mean to be without it. If in place of opening a valve we had to go to the woodshed or coalhouse and then build our fire-carry out the ashes-well, some of us I am afraid would be late reaching our offices and perhaps would miss our hot cakes for breakfast. One cubic foot of gas produced from the White Sand formation contains 1130 B.t.u. and weighs 47/1000 lb.; there are about 24,000 B.t.u. in 1 lb. of gas. Temperatures of over 3400 deg. Fahr. have been obtained with natural gas. Not only is it a superior fuel for the home but it has no equal for use in many large manufacturing industries, especially with the making of glass, pottery and open-hearth steel. In an open-hearth furnace, properly constructed, 5000 cu. ft. will melt one ton of steel. It requires 1/3 ton of bituminous coal gasified in a producer to do the same work, or about 40 gal. of tar or fuel oil, or 11,000 cu. ft. of by-product gas.

Jan 1, 1926

By F. W. Bowdish

Analysis of data on the equilibrium exchange of sodium ions from salt solutions for calcium ions, from various fractions of an oxidized calcareous iron ore from Lorraine, France, strongly suggests that the calcium may be attached to the solid by only one of its bonds. Nearly equal values were found for the equilibrium expression from data covering concentration ranges of 1000 fold for the salt and 235 fold for the ion-exchangeable calcium. Differences indicated between the exchangeable calcium contents of the slime and the sandy portions of the ore, as well as the equilibrium relationship itself, are of importance in the flotation of the ore. During an experimental program on the flotation of oxidized calcareous iron ores from Lorraine, France, ion-exchangeable calcium was found in the ore. Because this source of calcium ions, if not controlled, could thwart all efforts at flotation, an extensive study was made of the phenomenon. The part of that study reported here was to obtain data on the equilibrium established between ore solids and solutions of sodium chloride, and to analyze the data to try to understand better the physical chemistry of the exchange. The ore contains oolites of goethite and quartz grains embedded in a matrix consisting of calcite and a brown cement believed to be the residue from oxidation of the silicate minerals found in fresh unoxidized ore. When ground, a substantial fraction of the ore becomes a fine slime in which is concentrated more than half of the alumina content of the ore. It is believed that the alumina occurs as unidentified clay minerals with which most of the ion-exchange capacity of the ore is associated. A preliminary experiment on the exchange of ions from the ore for sodium ions from solutions of NaCl showed that calcium was about ten times as abundant as magnesium in the exchange solutions. Thus calcium was the predominant ion in causing difficulties with flotation, and it was the only one for which data was obtained in this study. It is believed that the omission of magnesium ion exchange from consideration does not invalidate the results. It is possible, however, that inclusion of magnesium in the analyses and calculations or its prior elimination from the samples would have improved the consistency of the results. EXPERIMENTAL Data about the equilibrium exchange of sodium from solutions for calcium from the solids were obtained using two different samples of material. The solids

Jan 1, 1963

By R. B. Toombs

The national and international importance of Canada's minerals and metals producing industry is reported. The growth of the Canadian industry is traced from 1945, through the period of rapid development of the early 1950's, to the consolidation and expansion activities of the late 1950's and early 1960's. Mineral production in Canada during 1963-including steel, nonferrous metals, and fuels -is reported. It is estimated that by 1970 the Canadian industry will produce $3.9 billion worth of metals, nonmetals, and fuels.

Jan 8, 1964

By H. R. Thresh

An oscillational vis cometer has been constructed to measure the viscosity of liquid metals and alloys to 800°C. An enclosed cylindrical interface surrounds the molten sample avoiding the free surface condition found in many previous measurements. Standardization of the apparatus with mercury has verified the use of Roscoe's formula in the calculation of the viscosity. Operation of the apparatus at higher temperatures was also checked using molten lead. Extensive measurements on five different samples of zinc, of not less than 99.99 pct purity, indicate i) impurities at this level do not influence the viscosity and ii) the apparatus is capable of giving reproducible data. The variation of the viscosity ? with absolute temperature T is adequately expressed by Andrade's exponential relationship ?V1/3 = AeC/VT , where A and C are constants and V is the specific volume of the liquid. The values of A and C are given as 2.485 x 10-3 and 20.78, 2.444 x 10-3 and 88.79, and 2.169 x 10-3 and 239.8, respectively, for mercury, lead, and zinc. The error of measurement is assessed to be about 1 pct. Prefreezing phenomena in the vicinity of the freezing point of the zinc samples were found to be absent. AS part of an over-all program of research on various phases of melting and casting nonferrous alloys, a systematic study of some physical properties of liquid metals and their alloys was undertaken in the laboratories of the Physical Metallurgy Division.1,2,3 The most recent phase of this work, on zinc and some zinc-base alloys, was carried out in cooperation with the Canadian Zinc and Lead Research Committee and the International Lead-Zinc Research Organization. One of the properties investigated was viscosity and the present paper gives results on pure zinc; the second part, on the viscosity of some zinc alloys, will be reported separately. Experimental interest in the viscosity of liquid metals has virtually been confined to the past 40 years. The capillary technique was already established as the primary method for the viscosity of fluids in the vicinity of room temperature; all relevant experimental corrections were known and an absolute accuracy of 1 to 2 pct was possible. Ap- plication of the capillary method to liquid metals creates a number of exacting requirements to manipulate a smooth flow of highly reactive liquid through a fine-bore tube. Consequently, the degree of precision usually achieved in the high-temperature field rarely compares with measurements on aqueous fluids near room temperature. However, the full potential of the capillary method has yet to be explored using modern experimental techniques. As an alternative, many investigators in this field have preferred to select the oscillational method. Unfortunately, the practical advantages are somewhat offset by the inability of the hydrodynamic theory to realize a rational working formula for the calculation of the viscosity. In attempting to overcome this restriction many investigators have employed calibrational procedures, even to the extent of selecting an arbitrary formula for use with a given shaped interface. However, where calibration cannot be founded on well-established techniques, the contribution of such experiments to the general field of viscometry is questionable. A critical appraisal of the viscosity data existing for pure liquid metals reveals a somewhat discordant situation where considerable effort is still required to establish reproducible and reliable values for the low-melting point metals. The means of rectifying this situation have gradually evolved in recent years. Here, the theory of the oscillational method has undergone major advances for both the spherical and cylindrical interfaces. The basic concepts of verschaffelt4 governing the oscillation of a solid sphere in an infinite liquid have been adequately expressed by Andrade and his coworkers.5,6 Employing a hollow spherical container and a formula, which had been extensively verified by experiments on water, absolute measurements on the liquid alkali metals were obtained. The extension of this approach to the more common liquid metals has been demonstrated by culpin7 and Rothwel18 where much ingenuity was used to surmount the problem of loading the sample into the delicate sphere. Because of the elegant technique required to construct a hollow sphere, the cylindrical interface holds recognition as virtually the ideal shape. On the other hand, loss of symmetry in one plane increases the complexity of deriving a calculation of the viscosity. The contributions of Hopkins and Toye9 and Roscoe10 have markedly improved the potential use of the cylindrical interface in liquid-metal viscometry. The relatively simple experi-

Jan 1, 1965

By J. B. Dilworth

OUTCROPS of coal have bees discovered is many localities is the Philippine archipelago, and practically all of the larger islands contain deposits of this mineral. Very little prospecting has been done to determine the value of the various coal-bearing areas, but so far as known, the largest and most promising fields are found : (1) is northern Cebu; (2) is the small island of Batan, a part of the province of Albay is southeasten Luzon; (3) is the somewhat larger island of Polillo, off the east coast of Luzon, and (4) is southern Mindoro, sear the small coast tows of Bulalacao. Northern Panay, south-central Cebu, and various localities is southern Luzon, Masbate, Negros, and Mindanao also afford evidences of the existence of coal-beds, the extent and value of which have not yet bees proved. The general position of these islands and districts is shows on the map of a portion of the Philippine Islands, Fig. 1. Some of these coal-fields have been known for many years (coal was discovered is Cebu 1827 and is Batas is 1842),1 and several futile attempts were made by the Spaniards to operate mines is these districts. But owing to many circumstances, chief among which were indifferent management, the political unrest of the islands, natural difficulties of transportation, and those inherent in the mining of steeply-inclined and somewhat irregular seams, no considerable output was ever obtained from any of these mines, and the fuel required is the many departments of industrial and political life has continued to be drawn largely from Australia and Japan. These conditions exist to a great degree at present, and though much interest is the coal-deposits of the Philippines

Jan 1, 1909

By A. W. Ruff

The seismic wave produced by an explosive is very important in blasting. A true understanding of the wave is only important when considering possible structural damage to buildings located near the blast, but it is also of primary importance when considering rock fragmentation. Because of the importance of the seismic wave to fragmentation, a finda-mental study of the seismic wave and its effect was made at the Cananea Consolidated Copper Co.'s mine at Cananea, Sonora, Mexico. Strain gages were used to measure the strain in the rock when nearby explosive charges were detonated. The variance in the circuit voltage caused by changes in the resistance of the strain gage was measured with an oscilloscope and recorded with a Polaroid camera. CONFINED DRILLHOLE CHARGES To record the seismic wave from a confined drillhole explosive charge, a gage was cemented to the bottom of a 4-in diam drillhole. The horizontal gage hole and nine horizontal charge holes were drilled perpendicular to the center line of the 2-39 drift and 4 ft above the floor. The gage hole was 29 in. deep, and the charge holes were drilled so that each bottomed 1 in. deeper than the gage hole. The gage was installed with its axis horizontal and parallel to the 2-39 drift. The charge holes had the following horizontal distances from the gage: hole 3, 3 ft; hole 4, 4 ft; hole 5, 5 ft; hole 9, 9 ft; hole 10, 10 ft; hole 14, 14 ft; and hole 15, 15 ft. Figs. 1 and 2 show the relationships of the gage and the charge holes. Charges of 80 pct special gelatin, which weighed 50, 100, and 150 g were exploded in the charge holes and the seismic waves were recorded. All charges were stemmed with 200 g of mud and detonated with an electric blasting cap. Fig. 3 shows the recorded seismic waves. The reflected components of the waves were too weak to be objectional on these records. Table I shows the data taken from the wave forms. The approximate average velocity of a wave with a 9-ft travel distance was 12,900 fps. Since different charge weights were used, it was necessary to scale the data. The scaled maximum compress ion-strain data and the scaled maximum tens ion-strain data are shown in Figs. 4 and 5, respectively. Figs. 6 and 7 show the strain-distance data from Figs. 4 and 5 converted to a 1-lb charge. The results showed that the wave consisted of an initial compression pulse followed by a tension pulse. The amplitude of the tension pulse approached the amplitude of the compression pulse as the distance between the gage and the shot increased. The decay rate of the seismic wave is very important in the evaluation of the blasting characteristics of a rock. When high-amplitude stresses are produced, as in rock fragmentation, the rate of decay is much more rapid than when small amplitude stresses are produced. In underground mine blasting, the burdens are usually not greater than 6 ft and the decay is very rapid. The rapid seismic-wave decay rate in the fragmentation range means that in practice, if the minimum weight of powder is used to break a specified burden, only a very

Jan 1, 1961

By S. R. B. Cooke, W. Philippoff, Donald E. Cadwell

[THE importance of contact angles in flotation has long been recognized, but little has been done to get quantitative relationships between the surface coverage of the mineral by the reagent, the length of the hydrocarbon chain, and the contact angle. It is well known that for a complete monolayer on the surface of a mineral the contact angle ? is determined only by the reagent&apos; and principally by the chain length of the hydrocarbon radical. Although for flotation the monolayer usually is regarded as being complete, early experiments of Wark and Cox2 showed that at very small concentrations of potassium ethyl xanthate the contact angle on galena changed in a continuous way from 0° to the equilibrium value of 60°. Further, Gaudin and Vincent&apos; showed a similar continuity using heptylic acid and sphalerite. This shows that with probably incomplete monolayers, ? varies with the degree of surface coverage. At the time these experiments were made it was impossible to measure the actual amount of surface coverage, especially since the decrease of the collector concentration in the liquor could be influenced by chemical side reactions. Through the use of the radioactive tracer method for the measurement of the amount of collector adsorbed on the surface of the mineral, Gaudin and Bloecher4 were able to determine accurately the actual surface coverage of dodecylamine acetate on quartz, but they did not measure any contact angles. It is believed that the relationship between the surface coverage and the contact angle is extremely important in flotation, especially as Gaudin and Bloecher showed that a 95 pct recovery is possible with a coverage of only 5 pct. Theoretical Considerations The work of adhesion W is the energy bound (in ergs per sq cm) when an interface is formed. It is determined by, the difference of the free surface energies (surface tensions) of the respective phases ?1 and ? 2 before contact and the interfacial free surface energy ?12 after contact. The definition of the contact angle permits the elimination of the unknown surface energy of the solid and hence the calculation5 of W from the surface tension of the liquid ? and the contact angle ?: [W = y (1 + cos ?)[1]] Consider a surface consisting of two components, identified as 2 and 3, 1 being the liquid. The amount of 2 in the composite surface is x, where 0 < x < 1. The respective contact angles with 1 and air are ? and ?3. The total work of adhesion of such a surface is the sum of the values of the components multiplied by their respective areas. A formal relation can be written: [W,,,=x•W2+ (1-x).WR[2] .] in which Wm is the work of adhesion of the composite surface. Eq 1 can be introduced into W2 and W3 but in the case of Wm some discussion is needed. If the two components are segregated, each component forming an integral part of the composite surface there is no physical meaning for a contact angle ?m, calculated from Wm, by using eq 1. If, on the other hand, the area of each patch of the components is small in comparison with, say, the diameter of the bubble used in measuring, it could be expected that ?m would have aphysical significance, because of the action of the surface tension of the liquid-gas interface tending to smooth out sharp corners. How small these patches would have to be is difficult to predict, but by using composite surfaces with microscopically]

Jan 1, 1952

By M. E. Wadsworth, T. D. Chatwin

The kinetics of sulfidization of hematite (Fe203) by H2S gas at various partial pressures have been determined over the temperature range of 170° to 500°C. The process was controlled by thin films of pyrite (FeS2) and troilite (FeS) which were protective and formed diffusional layers. At higher temperatures the thermodynamic drive to form FeS2 decreased, and consequently the rate of formation of FeS, decreased. Conditions for the development of thin layers of FeSz consisting of 10 to 100 atomic diameters are presented. Laboratory flotation results on synethetic ores indicate floatability identical to that of pyrite of normal xanthate flotation. The prospect of high-temperature sulfidization of metal oxides using H2S, S, or other sulfur bearing compounds is intriguing as a potential activation process for flotation since the thermodynamics are very favorable for a large number of systems. If the kinetic parameters are sufficiently well understood it may be possible to provide surface sulfide layers a few angstroms thick, thus imparting normal sulfide floatability characteristics to the oxide. For thin layers the total sulfur pick-up would be small except for very high surface area materials but in most cases this sulfur could be readily removed by roasting if necessary. The general reactions for the sul-fidization of metal oxide MxO, to a metal sulfide MpSq using H2S may be written for the three conditions py > xq; py < xq; and py = xq: A large thermodynamic advantage is obtained in many systems because of the relatively large negative free energy of formation of H,O compared to H,S. For the temperature range 2S° to 1500°C &apos; where AFOis the standard free energy and T is absolute temperature. As is evident from Eqs. 4 and 5, the free energy of formation of H ,0 is approximately 35 to 37 kilocalories per mole greater than that for H,S over broad variations of temperature. For oxide-sulfide systems as outlined above, sulfidization may be expected to occur for the conditions: Groups I and 111: that is, if the terms on the right are more negative than those on the left the reaction is expected to occur thermodynamically. The value hFg,(,) is included in Eq. 6 since hFLzs is based upon gaseous S2 rather than the normal reference state, orthorhombic sulfur. The

Jan 1, 1969

By M. R. TECK, N. Rudd, L. K. Thomas, D. L. Katz

The authors are to be congratulated for presenting the first comprehensive paper on the theory and practice of threshold pressure determination in connection with underground gas storage. It is of particular value since most previous experimental work on this subject has been proprietary to the commercial laboratories engaged in such testing and to their clients. This dlscussion is presented in amplification of the subject paper, not in criticism, and is based upon our experience with approximately 5,000 threshold pressure determinations. Our comments are directed primarily to the experimental procedures as described by Thomas et al. It should be noted that, while clay mineral-rich lithologies are the most common caprock materials, the samples used (Table 1) include low permeability sandstones and carbonates, but do not include shales or other formations in which clav minerals exert a dominant effect. While our experience on samples analogous to those investigated by the authors generally confirms their findings, we have found that even more rigorous experimental conditions must be imposed where clay minerals are the controlling factor. These additional conditions result from the well-known molecular character of the clay minerals themselves in which water is interlaminated with, and bonded to, silicate sheets, thus becoming an essential component of the molecule. In many clay minerals the character of the intersheet bonding, and thus the dimension of the lattice, is strongly affected by variations in the identity and concentration of cations present in the intersilicate water. On a supermolecular scale, adsorbed water films on particle or "flakes" of shale provide much of the cohesive force necessary to maintain mechanical strength. The thickness of these films is variable and inversely proportional to intergranular pressure within the dimensional limits involved in caprock investigation. The thickness of the intersilicate water layers may also be subject to pressure under some conditions. These considerations are reflected in several necessary modifications of the experimental procedures described by the authors. Two of these are, in our judgment and experience, of such importance that they cast real doubt on the validity of data obtained on argillaceous materials without their application. The very careful resaturation procedures proposed by the authors should give good results in connection with the relatively "inert" lithologies used in their experiments. Our experience suggests, however, that they would create more problems than they would eliminate if applied to argillaceous materials. 1. Drying of the sample at the temperature and for the duration indicated by the authors not only will dessicate the sample with consequent shrinkage cracking, parting along bedding planes, and even total disassociation in the case of fissile shales, but it may also alter the character of the clay minerals themselves — in some cases irreversibly. 2. Prolonged evacuation to 2 microns Hg further dessicates the sample and is even more effective in reducing the intersilicate water content. 3. Resaturation with water differing in pH or chemical content from that existing originally in the sample also serves to alter the nature of the sample, particularly its structure and strength. 4. Our experience has been that, even with the thorough precautions proposed by the authors, complete resaturation of very fine grained materials is rarely obtained. Yet our experience confirms the

Jan 1, 1969

By Jun Hino, P. G. Shewmon, P. A. Beck

THE investigations of Crussard,&apos; of Guinier and Tennevin,&apos; and of Dunn and Daniels," indicate that the subgrains formed in a cold worked and annealed metal are capable of growing at each other&apos;s expense during annealing, if the temperature of annealing is sufficiently high and the time is long enough. The results of Dunn and Daniels are particularly convincing in showing that subgrain growth is essentially the result of the free surface energy associated with the subboundaries. In subgrain growth, as in ordinary grain growth, energy is gained as a result of the decrease in total subboundary surface area per unit volume. Recently, Wood and Scrutton4 found that the rate of subgrain growth upon annealing increased very considerably, if simultaneously a creep strain was applied to the specimen at a low strain rate. Working with 99.98 pct pure fine-grained aluminum, these investigators found that the continuous X-ray diffraction back-reflection rings of material strained at room temperature remained continuous after heating for ten days at 250 °C. However, when heated at the same temperature under a stress of 1000 psi even for only three days, the formerly continuous X-ray diffraction rings broke up into numerous dots, which were fairly clearly separated from each other. The continuous X-ray diffraction rings were interpreted as indications of a very small subgrain size, not resolved by the X-ray diffraction method used. The breaking up of the continuous X-ray diffraction ring during annealing under stress was taken as an indication of a great increase in subgrain size, so that the individual subgrains could then be resolved. The effect of simultaneous strain at a low strain rate in accelerating subgrain growth, discovered by Wood and Scrutton and designated by them as "cell growth," is of fundamental importance. The experiments described in this note were carried out in order to confirm Wood and Scrutton&apos;s results by direct metallographic observation. Also, information was sought as to the minimum creep strain necessary to produce this effect. A fine grained high purity aluminum strip was prepared by alternate 33 pct rolling and annealing treatments for 1 hr at 350°C. Specimens cut from this strip were subjected to a relatively fast creep strain of 7.2 pct in 3.5 min at 300°C under a constant load initially corresponding to 1185 psi. The subgrains set up were large enough (about 0.015 to 0.03 mm) to be clearly observed (Fig. 1) at X200 magnification with polarized light, after electrolytic polishing and anodic etching, producing a fine oxide film." The corresponding X-ray diffraction pattern is shown in Fig. la. After the fast creep strain treatment a portion of the specimen was subjected to a creep strain of 8.3 pct in 44 hr at 350°C under a constant load initially corresponding to 320 psi. Another portion, annealed under the same conditions, but not strained, served as control specimen. The subgrain size of a typical area of the specimen annealed under strain and of the one annealed without strain is shown in Figs. 2 and 3 (X-ray diffraction patterns, Figs. 2a and 3a). Annealing without strain produced clearly observable subgrain growth (subgrain size: about 0.03 to 0.05 mm). The effect of simultaneous strain was to increase greatly the rate of subgrain growth (resulting in a subgrain size of approximately 0.05 to 0.13 mm), in accordance with Wood and Scrutton. In another experiment, the effect of the amount of simultaneous strain was studied. The initial subgrain structure was set up by fast creep, as described previously. The specimen was then heated at 350 °C under a constant load initially corresponding to 320 psi, as above, for 2.2 hr (0.24 pct strain), and 8.8 hr (0.58 pct strain). Comparison with the corresponding unstrained control specimens by means of X-ray diffraction showed that 0.58 pct strain definitely had an effect, but the effect of 0.24 pct strain was doubtful.

Jan 1, 1953

By G. R. Love, M. L. Picklesirner

THE use of color adds a new beauty, power, and versatility to metallography. This has been amply demonstrated in a number of public exhibits and on the walls of corporate, government, and university metallographic laboratories around the world. Indeed, in a number of cases, the color not only is of esthetic value but is scientifically essential to the competent examination of particular samples and systems. Optical strain analysis,&apos; determination of true grain size in U-A1 alloys: phase identification in Nb-base alloys,3 analysis of transformation rates in heat-treated Nb-Zr alloys,4 measurement of solidification segregation in cast Nb-Zr alloys,&apos; study of the intermediate phases in Nb/Sn diffusion couples,6 investigation of the oxidation kinetics at various surface orientations in single crystals,7&apos;8 and a number of other research efforts9&apos;10 would have been vastly more difficult without the extra clarity and distinction introduced by color—either the colors resulting from particular polarized light techniques or the interference colors obtained by oxidation. It is unfortunate that the beauty of colored micro-structures cannot be shared more widely, but the economics of publishing a technical magazine apparently prohibits color plates except under extraordinary circumstances. It is doubly unfortunate that no convenient, general method exists for communicating the information available in colored microstructures to the scientific community. True, in some instances the color changes observed are dramatic enough that direct black and white photography is adequate. In photoelastic stress analysis, several orders of interference fringes may be produced and it is frequently desirable to suppress the color effects (use monochromatic light) to simplify interpretation. On the other hand, relatively minute color variations may be readily detectable by eye, be of considerable assistance in interpreting a structure, and yet be enormously difficult to reduce to an unambiguous black and white print. In order to illustrate a possible compromise or solution to the above problems, we wish to show three black and white photographs of the same region of an Nb/Sn diffusion couple whose interpretation depends heavily upon use of color techniques. These micro-structures were obtained from a section through a rod consisting of commercial-purity niobium tubing filled with 99.995 pct Sn (melt-filled in 10"6 Torr vacuum). The composite rod, measuring 500 mm long, was bent into a hairpin shape and inserted into water-cooled copper grips in a vacuum high-temperature furnace. The rod was outgassed for 2 hr at a furnace temperature of 800°C and was further heated by self-resistance using a 2.2-kva ac power supply. The rod was raised to 1910°C over a 4+-hr period, held for 15 min, slow-cooled to 1500°C over a -hr period, and free-cooled to room temperature (all temperatures were measured with W5Re/W26Re thermocouple). Throughout the heat treatment the ambient pressure was kept below 8 x lo-&apos; Torr. Metallographic preparation of the sample was completely conventional except that it was necessary to extend the grinding steps to remove damage in the brittle NbsSn phase introduced by sectioning. No satisfactory chemical or electrochemical etch has been found for these diffusion couples; of those which have been tried, any that attack the niobium-rich phases at all attack the tin-rich phases disastrously. However, the final polishing steps did produce a slight relief effect and this, coupled with anodizing, yielded excellent clarity in the microstructures for direct observation. The anodizing voltage was chosen to give maximum change in color per unit change in composition. In this case, indeed normally, this maximum sensitivity occurred in the blue-to-red color range. The pure niobium tube wall anodized to a relatively bright blue

Jan 1, 1967

By AIME AIME

A CERTAIN area in the State of Indiana seems to be a breeding place for presidents and near president about eighteen miles southeast of Elwood is the little village of Daleville, and there, on April 9, 1890, John Robert Suman, newly elected President of the A.I.M.E., was born. It was not long before he migrated to California, however, where he went to the Los Angeles High School, then for two years to the University of Southern California, after which he went up to Berkeley

Jan 1, 1940