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By J. R. Bridge, D. A. Vaughan

The phase diagram of the Zr-H system over the range 0 to 65 atomic pet was determined by high temperature X-ray diffraction methods. Results show a eutectoid between a zirconium and the hydride phase. The eutectoid temperature was established at 560±10°C with a eutectoid composition of 42*3 atomic pet H. The hydride phase of the lowest hydrogen content is stable only above the eutectoid temperature, but is formed and retained in a metastable state during reaction of zirconium with hydrogen at temperatures below 560°C. One hydride phase is indicated that exists over the composition range 55 to 65 atomic pet H. RECENT increase in the industrial importance of zirconium has stimulated several investigations of the reaction of zirconium with hydrogen. Review of the literature on interpretation of absorption isotherms' ' shows that attempts were made to relate the observations to the room temperature hydride phases reported by Hagg.3 However, more recently Schwartz and Mallett' reported the existence of a new hydride phase, isomorphous with the lower hydride in the Hf-H system described by Sidhu.4 This phase was found adjacent to the metal in a diffusion gradient sample. In addition to the new phase, Schwartz and Mallett reported on only two of the five hydrides found by Hagg. Gulbransen" confirmed the existence of only three hydrides of

Jan 1, 1957

George B. CoRless, Chairman. Superintendent, Gulf Coast Division, Humble Oil & Refining Co., Houston, Texas. W. H. Geis, Associate Chairman. Geologist, Los Angeles, California. Benjamin C. Craft, Secretary-Treasurer. Associate Professor, Petroleum Enginecring, Louisiana State University, Baton Rouge, La. Executire Committee George B. Corless, Chairman. M. Albertson, Production Engineer, Shell Petroleum Corporation, Houston, Texas. D. R. Knowlton, General Production Superintendent, Phillips Petroleum Co., Bartlesville, Oklahoma. R. P. McLaughlin, General Manager, Dominguez Oil Fields Co., Los Angeles, California. Hallan N. Marsh, Production Engineer, General Petroleum Corporation of California, Los Angeles, California. Theron Wasson, Chief Geologist, The Pure Oil Co., Chicago, Illinois. Production Engineering M. L. Haider, Vice-chairman. Petroleum Engineer, Carter Oil Co., Tulsa, Oklahoma. Joseph Chalmers, DeBataafsche Pet. Maatschappij, The Hague, Netherlands. Emile HugUenin, Deputy State Oil and Gas Supervisor, Los Angeles, California. Carl E. Reistle, Jr., Petroleum Engineering Department, Humble Oil & Refining Co., Houston, Texas. Production J. TERry Duce, Vice-chairman. Geologist, The Texas Company, New York, N. Y. Basil B. Zavoico, Associate Vice-chairman. Geologist, The Chase National Bank, New York, N. Y. Engineering Research R. L. Huntington, Vice-chairman. Associate Professor, Petroleum Engineering, University of Oklahoma, Norman, Oklahoma. Economics Sidney A. SwensrUd, Vice-chairman. Assistant to the President, Standard Oil Co. (Ohio), Cleveland, Ohio. Refinery Engineering Walter Miller, Vice-chairman. Vice-president, Continental Oil Co., Ponca City, Oklahoma. 10

Jan 1, 1938

The first session of the Institute was held at the Smithsonian Institution, on Tuesday evening, February 22d. The members were welcomed to Washington and to the Smithsonian by Prof. Joseph Henry. President Holley responded to the cordial welcome of Professor Henry, and then read an introductory address on the subject of Technical Education. Following the discussion on President Holley's address the following persons, duly proposed and indorsed by the Council, were elected members and associates of the Institute : MEMBERS. Emile R. Abadie,. .. .. St. Louis, Mo. R. J. Anderson,.....Pittsburgh, Pa. Commander L. A. Beardslee,. .. Washington, D. O, Charles Bender,. .. .. New York City. Charming M. Bolton,. .. . Richmond, Va. Thomas E. Bowman,. .. . Silverton, Colorado. Calvin E. Brodhead,. .. . Bethlehem, Pa. M. L. Brosius,. .. .. . Lewistown, Pa. Harvey H. Brown,. .. .. Cleveland, Ohio. James A. Burden,.. .. . Troy, N. Y. J. P. Clemes,. .. .. . Sonora, Mexico. N. H. Cone,. .. .. . Nederland, Colorado. W. F. Durfee,.. .. . New York City. Robert Frazer, Jr.,. .. . Ashland, Pa, Joseph E. Galigher,.. .. . Bingham, Utah. William Golding,.. .. . Steel Works P. O, Pa. Samuel E. Griscom,.. .. . Pottsville, Pa. Gen. E. Burd Grubb,.. .. Beverly, N. J, Arthur R. Guerard,. .. .. Charleston, S. C. Edward Hart,.. .. .. Easton, Pa. Prof. Lewis M. Haupt,. .. . Philadelphia. E. S. Hawley,.....Buffalo, N. Y. John W. Hoffman,.. .. .. Philadelphia. Nelson P. Hulst,.. .. . Milwaukee, Wis. H. C. Humphrey,.. .. . Philadelphia. Ed. P. Jennings,.. .. .Ithaca, N. Y. B. F. Jones,......Pittsburgh, Pa.

THE first session of the Institute was held at the Smithsonian Institution, on Tuesday evening, February 22d. The members were welcomed to Washington and to the Smithsonian by Prof. Joseph Henry. President Holley responded to the cordial welcome of Professor Henry, and then read an introductory address on the subject of Technical Education. Following the discussion on President Holley's address the following persons, duly proposed and indorsed by the Council, were elected members and associates of the Institute : MEMBERS. Emile R. Abadie, - St. Louis, Ma. R. J. Anderson, - Pittsburgh, Pa. Commander L. A. Beardslee, - Washington, D. C. Charles Bender, - New York City. Channing M. Bolton, - Richmond, Va. Thomas E. Bowman, - Silverton, Colorado. Calvin E. Brodhead, - Bethlehem, Pa. M. L. Brosius, - Lewistown, Pa. Harvey H. Brown, - Cleveland, Ohio. James A. Burden, - Troy, N. Y. J. P. Clemes, - Sonora, Mexico. N. H. Cone, - Nederland, Colorado. W. F. Durfee, - New York City. Robert Frazer, Jr., - Ashland, Pa. Joseph E. Galigher, - Bingham, Utah. William Golding, - Steel Works P. O., Pa. Samuel E. Griscom, - Pottsville, Pa. Gen. E. Burd Grubb, - Beverly, N. J. Arthur R. Guerard, - Charleston, S. C. Edward Hart, - Easton, Pa. Prof. Lewis M. Haupt, - Philadelphia. . R. S. Hawley, - Buffalo, N.Y. John W. Hoffman, - Philadelphia. Nelson P. Hulst, - Milwaukee, Wis. H. C. Humphrey, - Philadelphia. Ed. P. Jennings, - Ithaca, N. Y. B. F. Jones, - Pittsburgh, Pa.

Jan 1, 1876

By M. R. J. Wyllie, F. Morgan, P. F. Fulton

The importance of formation factor, F, not only in electric logging but as a fundamental rock parameter has recently been stressed.',: The desirability of investigating the range of variation of the resistivity index exponent, n, in the relationship I = S ;", where I is the resistivity index and Sw the water saturation as a fraction of the void volume of a porous medium, has also been urged.3 The magnitude and variation of n with saturation and rock texture is a subject not only of theoretical interest but also one of prime importance in the interpretation of electric logs. A simple technique has recently been developed which enables both F and u to he measured with high accuracy and which may also find acceptance as a convenient method for the determination of irreducible saturation attainment in the restored state method of core analysis. Experience has taught that reproducible measurements of F are possible only if the resistance measuring electrodes are so arranged with respect to a plane face on a porous medium that they are able to make electrical contact with substantially all entry pores in that plane. In practice this may be achieved by using a platinized-platinum gauze electrode backed by some absorbent material (such as felt) which has been saturated with a fluid identical with that used to saturate the porous medium. Applicatiorl of pressure to the electrode and absorbent material then forces the gauze against the plane face of the porous medium and simultaneously squeezes saline solution through the meshes of the gauze. By this means the electrode is in continuous aqueous contact with all pores and satisfactory and reproducible low resistance contact with the porous medium is achieved. Clearly this method, although satisfactory for measurements of F, cannot be applied to the making of continuous resistance measurements on a porous medium while capillary pressure desaturation is being carried out. However, accepting the principle that for satisfactory results electrical contact must be made between a measuring electrode and all pores adja- cent to that electrude, methods of bringing electrodes into intimate contact with the surfaces of porous media were investigated. Two methods were ultimately found to be satisfactory: in the one, the metal electrode is formed on the required portion of the porous medium by the use of a metal spray gun, while in the second the electrode is painted on with an ordinary camel's hair brush. The first method has the advantage of permitting the use of any metal which can be sprayed, but has the disadvantage of requiring rather elaborate and expensive equipment. The second method is presently limited to silver electrodes although in principle other metals, e.g. platinum or gold, could be used. Moreover, the method is so simple and cheap, and has been found to be so satisfactory that it will be described in some detail. The core being investigated is cut into a right circular cylinder and is extracted and dried in the usual manner. The ends are then lightly painted with silver conducting paint* of the type used in printed electrical circuits. The quantity of paint used is not critical but the recommended, minimum compatible with entirely coating the core ends is recommended, particularly on the end that contacts the barrier. The core is then dried at atmospheric temperature for one hour or for shorter periods at any suitable elevated temperature up to about 110°C. It will be found that silver coatings so prepared are not only strongly adherent but also permeable and the core may be the core may be desaturated by the ordinary capillary pressure technique through one of the coated faces. The same permeability is characteristic also of thin metal coatings formed using the spray-gun technique. An ordinary Lucite capillary pressure desaturation cell has been adapted to a form suitable for measuring the resistivity of the saturated silver faced cores both at 100 per cent saturation (i.e., F) and at intermediate saturations down to the irreducible minimum. This has been achieved as follows: A Coors porcelain barrier, having a displacement pressure of c 30 psi was grooved across a diameter. Dimensions of this groove were c 1 mm deep and 1 mm wide at the top. The groove was then painted thickly with silver conducting paint, the paint in the groove being extended lightly over the edges of the groove for a distance of c 1 mm on each side. A 30 gauge silver wire was then arranged in the groove in a form of a spring bow, each end of the silver being held at diamet~ically opposite ends of the groove by means of plastic cement. The arc of the bow at its highest point was arranged to be a millimeter or so above the face of the barrier, while one end of the bow wire was led by means of a pressure-tight connection through the wall of the capillary pressure cell. The groove in the barrier was then Surrounded by suitably cut portions of Kleenex in the conventional manner so as to ensure capillary continuity from core to barrier, and the core placed on the barrier. The weight of the core distorted the silver spring bow and good electrical contact was thereby made between the outside of the cell and the lower painted silver electrode. Electrical connection to tile top painted silver

Jan 1, 1951

By M. R. J. Wyllie, F. Morgan, P. F. Fulton

The importance of formation factor, F, not only in electric logging but as a fundamental rock parameter has recently been stressed.',: The desirability of investigating the range of variation of the resistivity index exponent, n, in the relationship I = S ;", where I is the resistivity index and Sw the water saturation as a fraction of the void volume of a porous medium, has also been urged.3 The magnitude and variation of n with saturation and rock texture is a subject not only of theoretical interest but also one of prime importance in the interpretation of electric logs. A simple technique has recently been developed which enables both F and u to he measured with high accuracy and which may also find acceptance as a convenient method for the determination of irreducible saturation attainment in the restored state method of core analysis. Experience has taught that reproducible measurements of F are possible only if the resistance measuring electrodes are so arranged with respect to a plane face on a porous medium that they are able to make electrical contact with substantially all entry pores in that plane. In practice this may be achieved by using a platinized-platinum gauze electrode backed by some absorbent material (such as felt) which has been saturated with a fluid identical with that used to saturate the porous medium. Applicatiorl of pressure to the electrode and absorbent material then forces the gauze against the plane face of the porous medium and simultaneously squeezes saline solution through the meshes of the gauze. By this means the electrode is in continuous aqueous contact with all pores and satisfactory and reproducible low resistance contact with the porous medium is achieved. Clearly this method, although satisfactory for measurements of F, cannot be applied to the making of continuous resistance measurements on a porous medium while capillary pressure desaturation is being carried out. However, accepting the principle that for satisfactory results electrical contact must be made between a measuring electrode and all pores adja- cent to that electrude, methods of bringing electrodes into intimate contact with the surfaces of porous media were investigated. Two methods were ultimately found to be satisfactory: in the one, the metal electrode is formed on the required portion of the porous medium by the use of a metal spray gun, while in the second the electrode is painted on with an ordinary camel's hair brush. The first method has the advantage of permitting the use of any metal which can be sprayed, but has the disadvantage of requiring rather elaborate and expensive equipment. The second method is presently limited to silver electrodes although in principle other metals, e.g. platinum or gold, could be used. Moreover, the method is so simple and cheap, and has been found to be so satisfactory that it will be described in some detail. The core being investigated is cut into a right circular cylinder and is extracted and dried in the usual manner. The ends are then lightly painted with silver conducting paint* of the type used in printed electrical circuits. The quantity of paint used is not critical but the recommended, minimum compatible with entirely coating the core ends is recommended, particularly on the end that contacts the barrier. The core is then dried at atmospheric temperature for one hour or for shorter periods at any suitable elevated temperature up to about 110°C. It will be found that silver coatings so prepared are not only strongly adherent but also permeable and the core may be the core may be desaturated by the ordinary capillary pressure technique through one of the coated faces. The same permeability is characteristic also of thin metal coatings formed using the spray-gun technique. An ordinary Lucite capillary pressure desaturation cell has been adapted to a form suitable for measuring the resistivity of the saturated silver faced cores both at 100 per cent saturation (i.e., F) and at intermediate saturations down to the irreducible minimum. This has been achieved as follows: A Coors porcelain barrier, having a displacement pressure of c 30 psi was grooved across a diameter. Dimensions of this groove were c 1 mm deep and 1 mm wide at the top. The groove was then painted thickly with silver conducting paint, the paint in the groove being extended lightly over the edges of the groove for a distance of c 1 mm on each side. A 30 gauge silver wire was then arranged in the groove in a form of a spring bow, each end of the silver being held at diamet~ically opposite ends of the groove by means of plastic cement. The arc of the bow at its highest point was arranged to be a millimeter or so above the face of the barrier, while one end of the bow wire was led by means of a pressure-tight connection through the wall of the capillary pressure cell. The groove in the barrier was then Surrounded by suitably cut portions of Kleenex in the conventional manner so as to ensure capillary continuity from core to barrier, and the core placed on the barrier. The weight of the core distorted the silver spring bow and good electrical contact was thereby made between the outside of the cell and the lower painted silver electrode. Electrical connection to tile top painted silver

Jan 1, 1951

Since I have had the pleasure of watching the development of this process very closely, I feel that I ought to say a few words on the subject, although I cannot add much to what Mr. Roe has already said. I wish, however, to bear witness to the hard work, persistence and skill which have been exercised during the past two years, and which have so well deserved the success attained. Those of us who remember the history of the past efforts in this line, such as the rotary puddlers, in which also some of us had a part, can easily appreciate the problems involved, and may well be skeptical as to the outcome. Such, at least, was my frame of mind when the process first came under my notice. Now, after having seen every heat, but three, of the many made, it really seems to me that a process and plant for the mechanical puddling of iron has at last been developed which is practical, economical and successful. Of course I do not mean by this that either the process or the machines are developed to their highest point, technically or economically, but that, in my opinion, these goals are in plain view, and that the difficulties which remain are such as will be overcome by developing the skill of the operator through practice ;

Jan 1, 1903

By AIME AIME

FORMATION of a new company through the union of two familiar names in the mining and metallurgical world has just been announced. J. V. N. Dorr and E. L. Oliver have united the businesses and assets of The Dorr Company and Oliver United Filters, Inc., of which they are the respective heads, by the formation of the Dorr-Oliver Corporation under their joint management, and stockholders have approved the merger.

Jan 1, 1931

By Oscar Johnson

The industry has been canvassed for information on methods of handling grinding steel at milling plants, an important subject overlooked in most descriptive articles on milling plant arrangements. The data collected are offered in this paper as a guide to designers and planners who have loading and storage problems to solve. WITH capacities of milling plants expanding from a few hundred tons per day to many thousand, replenishment of grinding media is an important phase of mill operation. Information on this aspect of milling procedure, solicited from several mining companies, is summarized here. At International Nickel's Copper Cliff concentrator the normally strenuous job of changing rods is considerably simplified by the use of the Garrow rod charging machine, Fig. 1. The overhead crane, Fig. 2, brings a bundle of rods, weighing four to a ton, to the loading platform of the machine, positioned in front of the mill. The rods roll one by one down the slight incline of the platform onto a conveyor which sends them into the mill. A modified version of the Garrow machine, Fig. 3, is used at the Federal mill of St. Joseph Lead Co. An overhead crane places the portable steel structure in position in front of the discharge end of any one of the five 9x12-ft rod mills. It then raises a bundle of about twenty 3-in. rods to the discharge platform of the charging machine. The rods are 11 ft 7 in. long and weigh about 278 lb. By tripping a lever the operator allows one rod at a time to roll onto the inclined rollers. A slight push by the operator sends the rod smoothly into the mill. The Union Miniére du Haut Katanga rod charging machine, Fig. 4, is mounted on a pair of wheels at the forward end with swiveling castors at the back for steering it to position for use or storage. Wheels are equipped with locking brakes to maintain the machine in position while it delivers rods to the mill. The device is made in two parts. The first consists of the base, which carries the supporting wheels, grooved rollers, and drive. The other part serves as the rod deck, which can carry up to six 3-in. x 12-ft rods. A short boom built integral with the base reaches through the mill trunnion and delivers the rods into the mill barrel. Three grooved guide rollers ,are provided to receive the rods from the sloping charging deck. One rod at a time is fed to the rollers and thus delivered into the mill. Two of the rollers are driven by 11/2-hp motor through a V-belt drive. The third roller is driven off the first by a single V belt in a groove below the rod groove and on the same center line. Rods are delivered to the charger by an overhead crane in bundles of three to six as needed. The power is supplied by cables plugged into power outlets, suitably located near the rod mill discharge end. The Oliver Iron Mining Co. uses a rod charger, Fig. 5, suspended from a monorail by cables. It is constructed .of structural steel and has two decks, each capable of carrying five rods of 4-in. maximum diameter. The rods ride in grooved free-turning rollers. Legs extending down from the mill end of the mechanism act as supports when the unit is ex-

Jan 1, 1955

By H. M. Davis, T. S. Jones

A methodfor accelerating the reduction of a metal oxide by carbon monoxide is to incorporate in the reduction system a nonreducible oxide which has a strong affinity for carbon dioxide and will remove it from the product gases. The effectiveness of this method was investigated by veduction experiments on specially prepared powder mixtures of SrO-ZnO ("active'.) and SrCO3-ZnO (reference). Measurements at 750o and 677°C showed that the rate of reduction of ZnO by CO was as much as an order of magnitude greater in the presence of SrO. Under the experimental conditions at least as much CO2 as generated by veduction was absorbed when SrO was present. Enlzancernent of the veduction rate by SvO resulted from modification of' gaseous djfitsion processes. THE specific question posed in this investigation was whether the reduction reaction CO + ZnO - Zn(g) + COa [1] could be accelerated by incorporating strontium oxide into the oxide charge undergoing reduction. Provided the strontium oxide was active enough, it could remove carbon dioxide from the product gases of ( 11 and form strontium carbonate, thus modifying Reaction [ 1] to CO + ZnO + SrO = Zn(g) + SrCO3 [ 2] This study of the comparative rates of Reactions [ I] and [2] can be considered as a particular case of a general scheme for increasing the rates of reduction of metal oxides by carbon monoxide. The limits of applicability of this scheme are indicated in the simple thermodynamic analysis presented in the appendix. This analysis primarily dictated the choice of the system, CO-ZnO-SrO, employed in this investigation. In addition, it was thought that a study of this scheme by use of the CO-ZnO-SrO reaction system would be of special interest in view of indications in the literature1-3 that the gaseous reduction of zinc oxide is prone to rate control by diffusion in the gas phase. The distinction should be pointed out between this and other efforts to increase the rates of reduction reactions through the use of addition agents. Additions of a wide range of chemicals have been tried with de- grees of apparent success varying from slightly negative to highly positive. The reasons for making additions have included the use of salts to produce effects akin to catalysis,4, 5 the alteration of the microstruc-tural details of the reduction process (including solid-state diffusion),6-8 and the conversion of an en-dothermic reaction into one that is exothermic or autogenous.9-12 The means used to attempt alteration of the enthalpy change has commonly been to incorporate lime into the charge, so that heat is generated by reaction with either of the reaction products, carbon dioxide or water. The use of lime in this way makes endeavors such as that of Edstrom and Wiberg similar to the present one. Furthermore, the basic principle behind the present work has previously been set forth.13 However, a detailed investigation of the type of reaction described in this work does not appear to have been conducted. EXPERIMENTAL PROCEDURE From both conceptual and physical standpoints, Reaction [2] is to be considered as the sum of two reactions:

Jan 1, 1968

By R. E. Maringer, B. A. Wilcox, A. H. Clauer, J. H. Sovik

Internal friction measurements from 25° to 1100°C have been made on specimens machined from TD nickel bar. The use of miniature torsional pendulum specimens alloived damping measurements to be made on specimens whose axes were parallel to the original bar axis, at 45 deg to the bar axis, and at 90 deg to the bar axis. There was a marked difference in damping with varying specimen orientation, and this was related to the pronounced micro structural anisotropy of this material. Varying the microstructure by cold working plus re crystallization annealing also greatly affected the damping behavior. Recrystallization essentially removed the broad peak found at 400° to 650°C in as-received TD nickel, and in addition greatly lowered the background damping. DlSPERSION hardened metals such as SAP-type alloys (Al + AI2O3) and TD nickel (Ni + 2 pet ThO2) have been developed primarily to improve high temperature strength properties. There have been numerous damping studies on SAP-type alloys,1"9 and one of these6 showed that the damping capacity was greater than that of 99.5 pet pure Al from 25° to 600°C. Several preliminary observations on TD nickel10 and an experimental Ni-ThO2 alloy11 indicated that here, too, the damping capacity was quite high. A high damping capacity in TD nickel, combined with its relatively good high temperature creep strength, could provide an additional benefit for some high temperature structural applications. This work was undertaken to study the internal friction behavior of TD nickel bar over the temperature range 25° to 1100°C. In Ni-ThO2 and Ni-Cr-ThOz alloys, other properties such as steady-state creep rate,12 creep rupture life,12'13 modulus of elasticity,14 and ultimate tensile strength,14 are sensitive to orientation with respect to the primary working direction. Thus, in order to examine anisotropy effects in damping, studies were made on specimens machined with their axes parallel, at 45 deg, and transverse to the original bar axis. MATERIAL DESCRIPTION AND EXPERIMENTAL PROCEDURES The material used in this investigation was from the same £ in. diam TD nickel bar that has been studied previously.13'15 The structure typical of the as-received TD nickel is shown in Fig. 1, and additional details of the structure can be found in Refs. 13 and 15. Elongated grains are parallel to the bar axis and are about 10 to 15 u long and about 1 u in diam. This structure is very stable, since no recrys-tallization or grain growth occurred after annealing for 3 hr at 1300°C.13 The total ThO2 content was 2.3 vol pct and the particles ranged in diameter from 100 to 1000. The average particle diameter was 370Å and the mean planar center-to-center particle spacing was 2340Å. To examine the influence of grain and subgrain structure on damping, a section of TD nickel bar was swaged and drawn at room temperature from 1/2 in. diam bar to 0.040 in. diam wire (99.3 pct re-duction in area). The structure in Fig. 2 resulted after the wire was annealed for 3 hr at 1250°C. The recrystallized grains were much larger than the grains in as-received bar, but still showed considerable elongation in the direction of working. A high

Jan 1, 1970

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. 'The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,' In-AS,' and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956

By J. C. Scully, G. Sanderson

The electrolytic formation of y hydride in thin foils of Ti-5Al-Z.5Sn alloy and four Ti-A1 binary alloys has been studied by electron microscopy and electron diffraction. Two orientation relationships have been found: THE adsorption of hydrogen by titanium alloys from aqueous solutions has been widely reported. This can occur, for example, in both alkaline' and acidic2 pickling baths, in chemical polishing374 and electro-polishing Solutions,3,4 during cathodic polarization5" and under certain corrosion conditions,7,8 Etching reagents may also produce visible precipitates, sometimes after an aging period.9 During an investigation into the stress corrosion susceptibility of a titanium alloys by thin foil electron microscopy many observations have been made of hydride precipitation which has been deliberately promoted by techniques that are described below. The characteristics of hydride precipitation are reported and the observed crystallographic orientation relationships are discussed with reference to distortion in the titanium lattice created by the presence of the hydride. EXPERIMENTAL TECHNIQUE One grade of commercial titanium and five alloys were examined. Their composition and hardness values are shown in Table I. All the materials were in the form of thin sheet, 0.05 to 0.065 cm thick, which had been annealed after cold rolling. Foils suitable for transmission electron microscopy were made in two ways: a) by chemical polishing; and b) by elec-tropolishing. The solution used for chemical polishing was a mixture of 44 pct HF and 73 pct HNO3 in the volumetric ratio 2:3. During this polishing specimens were manually moved up and down in the solution. The reaction was veFy rapid, specimens thinning to foil thickness (2000A) in 5 min. Since chemical polishing solutions tend not to cause hydride contamination if they are kept cool3 no attempt was made to prevent the solution from becoming hot during the thinning operation. Electropolishing was performed at -30° C with a mixture3 composed of 295 cu cm methyl alcohol, 175 cu cm n-butyl alcohol, and 30 cu cm perchloric acid with an applied voltage of 40 v after chemically thinning specimens to approximately 0.017 cm thickness in a cool solution of 44 pct HF, 40 vol H2O2, and water in the volumetric ratio 1:6:3. EXPERIMENTAL RESULTS 1) Ti-5A1-2.5Sn Alloy. The Ti-5A1-2.5Sn alloy was severely contaminated by hydrogen during the chemical polishing. Foils obtained in this way contained large amounts of the y hydride phase. A typical micrograph is shown in Fig. l. The laths were identified as the hydride phase by selected-area diffraction of a large number of foils examined in a tilting stage that could be turned through 40 deg. Using the lattice spac-ings of the alloy obtained by X-ray diffraction as a standard the a value of the hydride was determined fromo the electron diffraction patterns to be 4.38 to 4.40A. The accuracy of this figure is only about ±2 pct. Further evidence of the identification was obtained by vacuum annealing chemically polished foils of the alloy at 500°C. This resulted in the dissociation of the hydride with the production of dislocations and possibly vacancy loops as shown in Fig. 2. The hydride

Jan 1, 1968

By Shun-ichi Satoh

A NEW method of treating steel by ammonia has recently been intro¬duced into the metallurgical industry, by means of which piston cylinders of internal combustion engines, shafts and other similar steel products can be made more resistant to wear than formerly. In 1929 the writer' published the historical notes and some experiments upon nitrification. He believes that the corrosion of nitrified steel is a matter of importance and worth studying; and as there have been few studies thereof, he has conducted experiments in this respect. L. Guillet,2 in 1927, reported corrosion tests made on nitrified and cemented steels with acid and salt solutions. In 1928, 0. Hengstenberg3 reported the high resistance of nitrified steel to water vapor and air. V. 0. Homerberg4 stated that nitrified steel has high resistance to water, air and salt solution; and G. Hagg5 studied nitrified layers of iron by means of the X-ray. Though F. Hanaman6 in 1913, measured the single potential difference of steel treated with ammonia at above 650° C., no one, it seems, has ever measured the single potential difference of the so-called nitrified steels having extraordinary hardness. The writer measured the single potential differences of nitrified special steels in various solutions with the object of studying the corrosion problem and, if possible, of knowing whether any new physical property would be caused by nitrification.

Jan 1, 1932

By Harvey T. Kennedy, Charles R. Olson

In many investigations of the performance of petroleum reservoirs the assumption is made that the liquid, if below its bubble-point pressure, is at all times in equilibrium with gas. On the other hand, observations by numerous investigators have indicated that gas-liquid systems including hydrocarbon systems, may exhibit supersaturation to the extent of many hundred psi in the laboratory. Up to the present, there has been no reliable data on which ti judge the actual extent of supersaturation under conditions approaching those existing in petroleum reservoirs. The work reported here deals with observations and measurements on mixtures of methane and kerosene in the presence of silica and calcite crystals. Bubbles were observed to form on crystal-hydrocarbon surfaces in preference to the glass-hydrocarbon interface or to the body of the liquid. Statistically, it was found that the number of bubbles formed per second per square centimeter of crystal surface was a function of the supersaturation only. and the function was evaluated graphically. Supersaturations were observed up to 770 psi, under which condition bubbles formed quickly and with considerable violence. With decreasing degrees of supersaturation, the frequency of bubble formation became less, until at 30 psi supersaturation and lower, no bubbles were observed to form, even though the observation at 30 psi was continued for 138 hours. It was found that silica and calcite crystals had identical effects, within experimental error, in accelerating the formation of bubbles, and that small amounts of water and crude oil had no effect on the results. It is shown that the maximum supersaturation that can exist in a reservoir may be calculated from the data presented and from the area of the rock surface. It is also shown that the number of bubbles formed in the reservoir, in order of magni- tude, may be calculated for any rate of pressure decline imposed on the reservoir by production. The bearing of the number and distribution of bubbles on reservoir performance is discussed. INTRODUCTION A liquid system is supersaturated with gas when the amount of gas dissolved exceeds that corresponding to equilibrium at the existing pressure and temperature. The degree of super-saturation may be conveniently expressed as the difference between the bubble-point of the mixture and the prevailing pressure. Thus, if a mixture having a bubble-point of 1,000 psi at a given temperature exists in single liquid phase at 700 psi at the same temperature. it is supersaturated to the extent of 300 psi. There are many examples of high supersaturations, mostly in aqueous solutions, reported in the literature. Thus, Kenrick, Wismer and Wyatt1 showed that water may be saturated with oxygen, nitrogen or carbon dioxide at 100 atmospheres, and the pressure reduced to one atmosphere without producing bubbles immediately. When liquids are in a state of tension, they may be considered as supersaturated at least to the extent of the tension. The tensile strength of water has been reported as 30 atmospheres by Meyer,1 60 atmospheres bv Budgett. 30 to 50 atmospheres by Temperley and Chambers,4,5 200 atmospheres by Dixon6. and 223 atmospheres by Briggs.7 Vincent8,9 determined the tensile strength of a mineral oil as 45 psi. Gardescu1 maintained pressures for short times in a model reservoir at 115 psi below the bubble-point. It should be noted that the high supersaturations observed were obtained on systems carefully purified to remove particles or surfaces which might promote the formation of bubble; These "nuclei" were considered as contaminants which interfered with the determination of a property of the liquid. In

Jan 1, 1952

By J. B. NEALEY

THE common method of shale mining, drilling, shooting and steam-shovel loading, is fast giving place to a comparatively new method which is purely mechanical. This machine is known as the shale planer and takes a cut from a very large face, 50 ft. or more in height. As shale deposits are usually stratified, the quality varying with the stratification, a very uniform product is obtained with this planer, for its "cut" is across the entire face, vertically. This planer was designed and built some 15 years ago by J. M. Powell, president of the Indiana Drain Tile Co., Brooklyn, Ind. Unevenness in mixing the material from the different layers in the shale deposit of this company was causing considerable fluctuation in the firing- shrinkage and color of the ware produced, thus lowering the quality. Some method of maintaining a uniform proportion was vital and this planer was therefore devised. Its capacity was approximately 175 tons daily: cut, mixed and loaded.

Jan 1, 1929

By Henry Faul

MEASUREMENT of radioactivity of rocks and ores has developed into a complete method of geophysical exploration. The problem falls into three natural categories: (I) surface radiation measurement in the field and underground; (2) radioactivity logging of drillholes; and (3) laboratory analysis of samples. Portable counters are used in the field for tracing radioactive formations and for quantitative estimates of radioactive content of surface rock. Wartime advances in battery design make it possible to construct small precision counters that can be carried easily. Even the smallest conventional diamond drillholes can be logged, and actual content of the radioactive element can be measured. The exact grade of very thin active layers or veins can be estimated only approximately. Samples may be analyzed for their alpha, beta or gamma activity, and beta assaying is the best suited to rapid routine operation. Simple calibration with standard samples is sufficient for rough work, but a density correction is necessary when greater precision is required. Samples with high emanating power should be fixed and stored for three weeks to reestablish the radium-radon equilibrium prior to precision assaying. Carnotite can be fixed by sintering or molding with plastics. Among the important new developments, a low-voltage Geiger tube has been designed recently, and crystal scintillation counters hold great promise for high-efficiency gamma-ray measurement.

Jan 1, 1947

By O. D. Gaither

This paper is an analytical study of the flow of fluids through small vertical conduits. Small conduits are defined as 11/4-in. nominal diameter tubing size and smaller, and approximately twice this area for annular conduits (i.e., 1- X 21/2-in. annulus and smaller). Experimental data are presented for the 1-X2-in. and 11/4- X 2%-in. annuli, and the I-in. and 11/4-in. tubing, since these represent the small conduit sizes and configurations generally encountered in oilfield applications. Data have been gathered for these conduits for single-phase water, single-phase gas and two-phase water-gas mixtures, with particular emphasis on high gas-liquid ratios. Water rates in excess of 2,000 BID and gas rates in excess of 2.5 MMcf/D, and two-phase flow ratios in between these two, represent the scope of the data gathered. Existing equations have been applied to predict flowing pressures and compared with experimental data. New correlations have been developed. INTRODUCTION The increased economic pressure on the domestic oil industry in the United States has constantly required the use of new techniques and equipment designed to reduce the cost of finding and producing oil and gas. Since tangible items are most readily apparent in economic analysis, the advent of lower-cost well completions was inevitable. One of the methods used to reduce costs which has received widespread attention is the slim-hole completion technique where tubing is used as the well casing and in which small conduits are used for tubing if necessary. Small conduits, defined by Kirkpatrick1 as "11/4-in. diameter nominal tubing and smaller for tubing flow and less than twice the 11/4-in. diameter nominal tubing internal flow area for annulus flow", have also found widespread usage as siphon strings for de-watering gas wells and as "kill" strings in deep high-pressure oil and gas wells. The growing use of small-diameter tubing has resulted in an increased need for development of improved methods to measure or predict flowing bottom-hole pressures since the physical dimensions generally preclude the use of subsurface-recording pressure gauges. Even in the cases where small bombs are available, the relatively high velocities encountered at nominal flow rates make it necessary to use excessive weight bars or special hold-down devices. Attempts to use recognized correlations to accurately predict flowing or gas-lift performance in wells equipped with small conduits have been generally unsuccessful. Insufficient field data were available to allow the development of a correlation on this basis, and an experimental approach was applied in an attempt to obtain a workable relation. The experimental approach used to obtain the data presented in this paper was actually a compromise between a field installation and a laboratory study. A test well 1,000 ft in length was used to obtain flow data on single-phase liquid, single-phase gas and two-phase water-gas flowing mixtures. Liquid rates up to 2,200 B/D and gas rates up to 3 MMcf/D were used in the single-phase flow studies. Two-phase flow rates from 100 to 600 B/D with gas-liquid ratios from 500 to 8,000 cu ft/bbl were recorded. Experimental data were obtained for single- and two-phase flow through 1-in and 11/4-in. nominal tubing, and through the annuli between 1- and 2-in. and 11/4- and 2%-in. nominal tubing strings. Experimental results for the two-phase flow are compared to the Poettmann-Carpenter correlation2 which is widely used as a comparative standard for development of multiphase flow predictions in flowing and gas-lift wells. Correlations developed by Tek,3 Baxendell and Thomas" were also investigated. The experimental data recorded herein fell in between the two flow regimes as defined by Ros," and this correlation also failed to yield satisfactory results. The fact that existing correlations failed to confirm the experimental data led to the need for development of a new correlation. Although a two-phase flow study was the primary objective of this investigation, data were also recorded for single-phase flow of water and gas, and constants were developed relating to pipe roughness and equivalent diameters for annular flow. These single-phase studies assisted materially in the development of certain of the two-phase flow results. Considerable previous work has been published which presented relationship of surface measurements to bottom-hole condition. The works of Buthod and Whiteley,6 Jones,' Poettmannb and the Texas Railroad Commission" are classic examples of the successful use of mathematical relationships which allow acceptable predictions of subsurface pressures, when gas is the flowing fluid. Darcy and others have derived relationships which may be used with minor modifications to predict subsurface flowing conditions in injection and water-supply wells. As previously stated, the application of the single-phase flow relationships

By P. E. Chapman, J. E. Worthington, I. T. Kiff

Increases in the price of gold starting about six years ago, and rapid fluctuations since then, have created a substantial popular interest in the noble metal. Gold prospecting had been at a low ebb since the end of World War II in most of the United States, except for a flurry of activity in Nevada after the Carlin and Cortez discoveries. The last few years, however, have seen a great awakening of interest in gold exploration as well as an opportunity for education for many explorationists in the geology and other vagaries of gold deposits. The writers have participated over the last few years in a search for gold deposits throughout the United States. This search was greatly influenced by the geologic studies of Dr. William Spence at the Haile gold mine in South Carolina, as reported in a companion paper. Spence's studies resulted in definition of a geologic model that has proven useful in a number of other geologic environments in the United States. These programs were all carried out under the auspices of Cyprus Mines Corp. and permission by Cyprus to present these results is gratefully acknowledged. The writers, however, reserve for themselves all responsibility for the results and conclusions. The exploration program to be described began in the southeastern United States. Spence's studies provided a reasonable basis for interpreting and understanding the geology of the Haile deposit, and also provided a means for predicting additional occurrences. This concept was then expanded to other gold occurrences in the Piedmont, and became an effective tool for evaluating other prospects. Finally, it became evident that the concept could be applied in some western gold districts. The following discussion will then include descriptions of other Piedmont examples and a few western districts that also appear to fit the pattern.

Jan 1, 1981

By C. K. Leith

In discussing the subject of mineral exploration, one is tempted to resort to reminiscence. I could tell of many missed opportunities, but I propose rather to outline certain changes in the methods and conditions of exploration which present new problems to the mineral explorers of today. Our subject might appropriately be called The Passing of the Old Time Prospector. The first question that presents itself is whether the job of mineral exploration is not already pretty well finished. The current market surplus of most minerals and the present overcapacity for production, with their attendant financial troubles, naturally raise the question whether the accumulation of reserves has not gone far enough for the present, and whether further exploration should not be left to some future time when consumption shall have caught up. Unquestionably we have gone far in the conquest of our physical environment, and the fear of shortage of minerals is less than formerly. For the time being there is no great need of further supplies for the world as a whole of many of the great essential minerals, coal, oil, copper, zinc, silver, and others. For a few minerals, such as gold and lead, the known future world supplies are not yet large enough. For all minerals the distribution is so unequal among the nations that exploration will continue in deficient areas in the attempt to make nations self-supporting.

Jan 1, 1932