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By H. W. Young

DEVELOPMENT of high-tension outdoor substations during the past few years has been due primarily to economic reasons. The demand for power in small communities could not be met with the conventional and 1 FIG. 1.-33,000-VOLT STEP-UP OUTDOOR AIR-BREAK SWITCH AND SUBSTATION INSTALLATION OUTSIDE OF A POWERHOUSE GENERATING AT 2300 VOLTS STEPPING UP TO 33,000. TWENTY-ONE COAL MINES ARE SUPPLIED FROM LINES LEADING FROM THIS INSTALLATION. comparatively expensive indoor types unless the rate for service was materially increased. That the various problems incident to development have been solved successfully, it is only necessary to point to the

Jan 9, 1919

By Paul H. Lu

Methods and results of measuring three basic parameters for ground stability control, ground pressure, strata movement, and geomechanical properties of mine rock are presented in this paper. It is found that these parameters can be measured in situ by simple and practical techniques with nonsophisticated and inexpensive instruments. Specifically, a drillhole dilation technique employing a cylindrical hydraulic borehole pressure cell (CPC) was used to determine the modulus of rigidity. Premining ground pressures were determined by pressure convergence tests with a combination of one CPC and two pre-encapsulated flat hydraulic borehole pressure cells (BPC) installed in a single drillhole. Abutment pressures and pillar loading were monitored with BPC's. Differential strata movements and bed separations were measured with self-recording 10-anchor-point extensometers. Roof-to-floor convergence was measured with self-recording convergence meters. Some applications of these in-situ-determined parameters to mine design and ground stability control are also discussed.

Jan 1, 1984

By R. Laird Auchmuty

The A. I. M. E. Subcommittee on Bituminous Mining has been trying for several years to secure the information that was collected by the Marquette Cement Manufacturing &. on the subsidence of its property caused by mining coal beneath it. The Marquette company was willing to have these data used, but it was impossible to obtain them because the records had been filed away. About two years ago these records became available and the engineering data presented herewith were compiled from them by R. L. Auchmuty, assisted by L. E. Young, who was connected with the collection of the information. On account of the cost, it is impossible to reproduce all of the data here, although the original information is on file with the records of the Committee on Ground Movement and Subsidence. The accompanying charts show representative and average data and give only the engineering information with enough description to tell how it was obtained. It is hoped that all of those connected with the original case will participate in the discussion that this will bring forth. Howard N. Eavenson, Chairman, Subcommittee on Bituminous Coal Mining. PRobably the most complete records of subsidence due to coal mining in the United States are those compiled by the Marquette Cement Manufacturing Co. at LaSalle, 111. These records, covering a period of more than three years, were compiled and used as evidence during the suit of the Marquette Cement Manufacturing Co. vs. the Oglesby Coal Co. at Oglesby, LaSalle County, Ill., in which the cement company successfully endeavored to stop the coal company from mining under its property. Fig. 1 shows a typical section of the geological formation. The cement company was mining the LaSalle limestone which lies about 125 ft. under the surface. The limestone is 30 to 35 ft. thick and underlain by about 15 ft. of shale. The cement company was mining about 20 ft. of the limestone, and in some places 10 to 12 ft. of the underlying shale, by the room and pillar method. The mining of the limestone always preceded the mining of the shale. The coal company was mining by longwall advance methods the NO. 2 seam of coal 42 in. thick underlying the limestone bed by 435 to 470 ft. The coal mine, a very old one, had largely mined out its original property

Jan 1, 1931

By Michael B. Bever, Carl F. Floe

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

By Carl F. Floe, Michael B. Bever

The solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to I300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. Review of Previous Work The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar5 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwasé3 reported large hydrogen solubility values for several compositions of copper-tin alloys, which appear to be in error.

Jan 1, 1944

By Walter Lee Brown

One of the characteristic steps in the march of modern scientific progress is the substitution of improved time-saving and labor-saving appliances for the antiquated and, in most cases, inconvenient forms of chemical and physical apparatus used by the earlier experimenters. This fact is strongly impressed upon us when we consider the question of the employment of illuminating-gas as a source of light, heat and power. Concerning its value as a light-producer, let the record of the past three-quarters of a century speak for itself. As a factor for power, we have evidence of its efficiency in the shape of the gas-engine. But its adaptability as a medium of heat, is the feature to which I wish to call attention, and in a special direction, viz., the assaying of ores. Gas assay-furnaces have been known and used for some years, but not to any very great extent, in this country at least. Therefore no apology on my part is required for the description I now give of a complete gas assaying-plant. The illustration accompanying this paper is a faithful representation of the group, as it was designed by, and arranged for myself, and appears in actual running order in my laboratory to-day. Its duty is to do roasting, crucible-fusion, scorification and cupellation. The furnace at the left is for roasting sulphurets or other ores for experimentation or actual work. It is what is known as a Fletcher No. 163, and consists of a fire-clay body strapped with sheet-iron bands, and a burner (No. 16, Fletcher). The opening at the top

Jan 1, 1885

By J. Lyndon Rosenblad

This chapter describes the development of a rocklike model material for use in tests with a rock-blocks model to investigate the failure mechanism of a discontinuum. In order to provide reliable results, the model material must be characteristic of natural rock and obey the laws of similitude. Initially, the development of such a material does not appear to be a difficult problem. Only when one undertakes such a task does he realize how little is actually known, and that there is considerable work yet to be done. A material that simulates rock in all of its physical properties probably will never be developed. There is now and probably always will be room for improvement. Improvement is needed not only in the component materials but also in the technique of preparation. The material developed and subsequently described in this chapter simulates rock in general and a schistose gneiss rock in particular. The material possesses many rocklike physical properties not found in previously used model materials. One of the most significant improvements of this material is that there is an increase of Young's modulus with an increase in confining pressure as determined by triaxial compression tests. A change in the usual procedure of material preparation was used to develop this material and is also described. MODEL MATERIALS USED IN THE PAST Intact Materials Numerous materials have been used by investigators in models in the past to simulate a wide range of prototype materials. Some of the materials used include cork, plastic, concrete, plaster of Paris, portland

Jan 1, 1972

By James E. Berryman

A method is presented for calculating the pressure depletion performance of a gas-condensate reservoir from the original reservoir fluid composition using the laboratory determined pressure-production history and retrograde liquid accumulation as guides. Equilibrium vaporization ratios for this calculation were modified from published data until the calculated dew point pressure and retrograde liquid accumulation agreed with the values observed in the laboratory. The calculated results are compared with the produced gas composition determined by low temperature analysis during constant volume laboratory experiments of pressure depletion behavior. This comparison shows that the calculation procedure is adequate for determination of gas phase composition. Data from field separation tests in low temperature separators are presented which verify the applicability of published equilibrium vaporization ratios for a wide range of separator conditions. INTRODUCTION A reliable prediction of the pressure depletion performance of a gas-condensate reservoir is necessary in determining reserves and evaluating field separation methods. The predicted performance is also used in planning future operations and studying the economics of projects for increasing liquid recovery. Because the flow of fluid in a volumetric gas-condensate reservoir is usually single phase flow, the pressure-depletion per-formake is primarily a function of the phase behavior of the reservoir fluid. The properties of a gas-condensate system of major importance are: (1) compressibility factor at reservoir temperature and pressure; (2) dew point pressure; (3) composition changes of the vapor phase with pressure depletion; (4) recovery of original in-place hydrocarbons at any pressure; and (5) retrograde condensate accumulation. These properties are most generally determined by a pressure depletion-type experiment on recombined separator gas and liquid samples in the laboratory. ldeally the pressure-depletion performance can be calculated from the composition of the original reservoir fluid if the reservoir temperature and initial pressure are known.1,2,3 It has been reported "... comparison of such computations with depletion-type ex-periments on recombined samples in the laboratory have yielded results that appeared to be entirely adequate.". The success of such calculations is determined by the equilibrium vaporization ratios chosen, especially those for the higher boiling point hydrocarbons. It is the purpose of this paper to present a method for computing the change in composition of the vapor phase during pressure depletion by production using laboratory determined properties of the system to guide the calculation and to illustrate the use of the method with data from the Cockfield "D" sand of Washington field, St. Landry Parish, La. Results of field tests and laboratory analysis are included. As a result of this reservoir fluid study, a cycling program has been evaluated, the fidd has been unitized, and the cycling started in July, 1956.

Jan 1, 1958

By J. A. Ede

The object of the writer is to call attention to a rather unique aggregation of economic products distributed over a line of succeeding formations about 3 mi. long, to be seen within a few miles of La Salle, Ill. Fig. 1 is an ideal section of the stratification exposed and exploited along a distance of 3 1/5 mi. in a southwesterly direction from the quarry of the Utica Hydraulic Cement Co. located near the historic site of Kaskaskia village to the Oglesby shaft at Oglesby. No attempt has been made to cover the whole field, special mention only being made (with the exception of two places) of the operations found along the course or parallel to the direction assumed in the ideal section. I have used Fig. 2, after J. R. Bent and De Witt Kelly, to locate the relation of the La Salle anticline to the coal mines of this district and to show the operation of No. 1 and 3 mincs of the Illinois Zinc Co. Anticline and the Rock Formations Owing to the structural deformation between La Salle and Utica, the older rocks of the state are exposed to the surface along the northern embankment and the bottoms of the Illinois River valley near the latter place. At; the Illinois Zinc Co. works, Sec. 16, Tp. 33, R 1, a well for water mas sunk 1828 ft. and samples taken every 10 ft. of the ground penetrated; duplicates were sent to Mr. Cady of the Illinois Geological Survey. A general compilation or synopsis study of this section is here presented. As the well is over 1 mi. west of the Western limb of the anticline, the section affords some reliable data. These samples were studied and interpreted by H. M. DuBois as Lower Magnesian, and by G. H. Cady as the Lower Magnesian. The results are given in Fig. 3. The most interesting geological feature of this district is the La Salle anticline. In 1865, Leo les Quereux, looking at Split Rock, asked how it happened that the upper coal measures overlie strata of the Lower Silurian and what has become of the formations which are generally found intermediate—the Upper Silurian, the Devonian and sub-carboniferous, and the lower member of the coal measures?

Jan 1, 1920

By AIME AIME

THE session on milling methods on Monday afternoon.* with G. H. Clevenger, chairman of the Mining Methods Committee presiding, was well attended. However, none of the authors of the papers presented were present except Messrs. Taggart and Ince. The paper on "Elements of Operations of the Pneu¬matic Table," by Messrs. Taggart and. Lechmere-Oertel, was presented by Professor Taggart as was the paper on "Calculations in Ore Dressing," by Luyken and Bierbrauer, due to the absence of the authors.

Jan 1, 1929

By I. R. Kramer

The delay time for single crystals of iron, zinc, and pre-strained aluminum was measured under conditions of high-speed deformation. The delay time of aluminum was found to be affected by the orientation of the crystal. Under the dynamic conditions employed, tile calculated "activated volume" term appears to be very small for the three metals studied. IN a previous paper,1 it was shown that under dynamic testing conditions at 78° K, there was a delayed yield in single crystals of aluminum and copper which had been cold-worked prior to testing. The experimental results also indicated that the delay-time effect was not due to the interaction of dislocations with impurity atoms or vacancies, but rather to a dislocation-dislocation interaction since aluminum which has not been prestrained shows no delay-time phenomenon. In this paper, some data are reported on the effects of orientation on the delay time of aluminum single crystals; the delay time of zinc single crystals saturated with nitrogen and the delay time of iron single crystals also were measured. EXPERIMENTAL PROCEDURE Aluminum (99.997 pct) and zinc (99.999 pct) crystals, 1/2 in. in diam and 8 in. long were grown by the Bridgman technique. The iron single crystal was supplied by Dr. R. Maddin. The zinc crystals containing nitrogen were prepared by melting high-purity zinc in a graphite crucible and the nitrogen was introduced by additions of ammonium chloride. The liquid zinc was then drawn up into glass tubes of 1/2 in. diam and allowed to solidify. The rods were cooled to room temperature before the transfer to the mold for conversion into single crystals. The orientation of all specimens was determined by the Laue' back-reflection technique, Fig. 2 and Table I. To prepare for the delay-time measurements, the crystals were cut with a fine jewelers saw and the ends carefully machined. The specimens then were electrolytic ally polished to remove the cold-worked metal, mounted in a special fixture and hand-lapped. As a final step, the crystals were annealed in evacuated tubes. Specimens of aluminum crystals, Nos. 24 and 26, were compressed 0.5 and 2 pct, respectively, in the direction of the later impact. The zinc specimens were aged at 50°C for 15 min, In the case of iron, only two specimens could be obtained. To obtain sufficient data, it was necessary to resort to a reaging treatment. After each delay-time test, the specimens were aged at 65° C for 100 min. This treatment, according to Clark,2 is sufficient to restore the original delay time. It is believed that although the specimens were plastically deformed approximately 10-4 pct, after each test the delay-time values are reliable. The delay-time measurements were made in an apparatus similar to that described previously.' Single crystals approximately 1 in. long and having a diameter of 1/2 in. were placed in a pendulum which consisted of a bar 1/2 in. in diam and 8 ft long, designed with a crystal holder to accommodate the specimen at low temperatures. The crystal was held at a position 2 ft from the front part of the pendulum. This portion of the apparatus was supported on a fine molybdenum wire. A projectile bar of the same diameter and length comprised the other portion of the apparatus. This bar was supported on

Jan 1, 1962

By D. I. Bardos, A. M. Bardos, Paul A. Beck

The approximate effective silicon radii in ternary Laves phase alloys with transition elements and silicon were found to range between 1.16 and 1.21A, i.e., considerably smaller than the atomic radius calculated for elemental silicon. The atomic radii were found to increase with the size of the transition element atoms in the structure. It has been noted by Aronsson1 that silicon in solid solution in iron, cobalt, and nickel has an effective CN 12 atomic radius of approximately 1.20Å, a value very much smaller than the CN 12 radius of 1.34Å derived from the interatomic distances in elemental silicon.7 The unusually short metal-silicon interatomic distances in transition element monosilicides and disilicides have been also pointed out by various investigators.1 A similar tendency was observed by Nevitt in Cr3O type silicides.2 Recent work on Laves phases in ternary systems of silicon with transition elements4"8 suggested that extensive Laves phase fields may occur in such systems.8 It has been pointed out by Laves7 that the MgCu2 and MgZn2 type structures lend themselves particularly well for the determination of the effective radii of the component atoms. In these AB2 phases the B atoms are arranged in close packed straight lines, and their distances are related in a simple manner to the lattice parameters.8 The present work was undertaken in order to find out whether or not the B transition element in such AB2 Laves phases can be replaced to an appreciable extent by silicon. In cases where extensive substitution proves to be possible, the "average atomic radius for the B site" at various silicon contents was to be determined, and the effective atomic radius of silicon calculated by extrapolation to complete replacement of the B component by silicon. The following ternary systems were studied: Ti-Mn-Si, Ti-Fe-Si, V-Co-Si, V-Ni-Si, Nb-Fe-Si, Nb-Co-Si, Ta-Fe-Si, Ta-Co-Si, and Mo-Fe-Si. In all of these alloy systems, the Laves phase solid solutions were found to extend over a considerable range of silicon content. As previously reported,4"8 in the V-Co-Si, V-Ni-Si, and Mo-Fe-Si ternary systems Laves phases do occur, even though there are no corresponding binary Laves phases. In stabilizing the Laves phase, silicon acts as if it were decreasing the effective electron concentration of the alloy.8 A more detailed study of the boundaries of the Laves phases in the V-Co-Si and V-Ni-Si systems has been made and will be published elsewhere. In both cases, the elongated Laves phase fields extend parallel to the B-Si side of the composition triangle, clearly showing that silicon is substituting for cobalt, respectively, nickel over a wide range of compositions. The binary Laves phases NbCo2 and TaCo2 have the cubic MgCu2-type structure. It was found that, in both ternary systems with silicon, again the MgZn2-type hexagonal Laves phase is stabilized and that this phase extends to high-silicon contents. In each ternary system at least three Laves phase alloys of the composition A(B1_xSix)2 were used, x here denoting the fractional substitution of the B-transition element atoms by silicon. The alloys, listed in Table I, were prepared by arc melting in argon. Each specimen was water quenched after a homogenizing anneal of 3 days at 110(FC, except for the Mo-Fe-Si alloys, which were annealed at 1200°C. Metallographic examination showed that most of the homogenized alloys consisted of a single phase, although some had minor amounts of a second phase, as shown in Table I. X-ray diffraction patterns were prepared using an asymmetrical focusing camera of large resolution and Fe Ka radiation. The patterns were indexed, and the lattice parameters of the hexagonal Laves phases were determined from the available diffraction lines of highest indices: (213), (205), and (313). The lat-

Jan 1, 1963

By J. P. Neumann, Y. A. Chang

Lattice parameter measurements of the hcp phase in the system Ag-A1 near the stoichiometric composition Ag2Al were carried out for specimens quenched from 825°K, annealed for 10 days at 453°K, and annealed for 100 days at 413°K. The three heat treatments resulted in the same lattice parameters at room temperature. None of the specimens showed any superlattice lines. The lattice parameters of this alloy were also measured at temperature from 77° to 750°K. An anomaly in the temperature variation of the lattice paramete.rs occurs in the region near 400°k, which may be associated with local ordering. FROM measurements of the diffuse scattering of X-rays, it is known that the [ phase in the system Ag-A1 near the stoichiometric composition Ag2A1 ex- hibits a considerable degree of short-range order at room temperature.' Moreover, based on the position of the short-range order peaks a superlattice model had been proposed in the same study and it was suggested that lowering the annealing temperature to 420°K might result in long-range order. In the present study, the diffraction patterns and the lattice parameters of three differently heat-treated specimens, i.e., quenched from 825°K, annealed for 10 days at 453°K, and annealed for 100 days at 413°K, were determined from 77" to 750°K. The purpose of these measurements was to investigate 1) whether long-range order could be established by prolonged annealing and 2) whether the lattice parameters at room temperature depended on the heat treatment, since it had been proposed earlier2 that the lattice parameters in this phase are related to the atomic arrangement. 1) EXPERIMENTAL TECHNIQUES Silver and aluminum, both 99.99 pct purity, were melted in a zirconium oxide crucible under helium in

Jan 1, 1969

By R. H. Maes, R. E. de Strycker, J. J. Jacobs

A simple method, based upow density measurements, has been perfected in order to determine the critical temperature of liquid miscibility gaps. Applied to the Pb-Cu system, it yielded a value of 980"C for the critical tempevature of the miscibility gap in this system. In the Pb-Cu-As system, the immiscibility between lead and coppev evolves towards a miscibility gap be-tween lead and copper arsenides; the liquation temperatures were determined joy different avsenic contents and values up to 1065°C were found. Combining these results with those given by the clzemical analysis of liquid samples taken at dqj.event temperatures, it has been possible to make a cowzplete determination of the liquid miscibility gap in this ternary system. In the Pb-Cu-Fe-As system, a ternary miscibility gap has been discovered; for some compositions, the molten and slowly cooled alloys separated into three layers: an Fe-As alloy, a Cu-As alloy, and a lead-rich layer. ThE Pb-Cu-Fe-As system is of interest for the study of the behavior of speiss or arsenical alloys in the lead blast furnace. The speisses produced in lead metallurgy generally have complex compositions, but they may be considered, in a simplified way, as a mixture of copper, iron, nickel, and cobalt arsenides; there is often an excess of metallic constituants, and lead is also present. Speisses liquate from lead at various temperatures according to their composition; according to industrial experience, iron speisses are already distinctly separated from lead bullion at temperatures of the order of 1100°C, whereas copper speisses only begin to liquate from lead at much lower temperatures, near their solidification points, which were never accurately determined until now. Besides these considerations of practical interest, the present study is of importance for the knowledge of liquid miscibility gaps. Particularly the data of the literature about critical temperatures of liquation are incomplete and present sometimes considerable disparities; a method has been perfected in the present work to determine these temperatures with accuracy. MISCIBILITY GAP OF THE LEAD-COPPER SYSTEM Review of Literature. The generally admitted outline of the Pb-Cu equilibrium diagram is shown by Fig. 1. This figure, with its numerical indications, is taken from the review of Hansen and ~nderko;' compositions are given in weight percent, as will be the case in the remainder of this paper. Between 36 and 87 pct Pb, Pb-Cu alloys separate into two layers, in the liquid state. The critical temperature of liquation has been much disputed in earlier studies, where values up to 1500°C were claimed; but a reliable study of ~ohnen,' based upon differential thermal analysis, gave a value of 990°C; this rather low value was verified by a recent study of Schiirmann and Kaune? based upon thermodynamical properties of the Pb-Cu alloys, which predicted a value of 1002°C. Liquid miscibility gaps were also studied by means of chemical analyses. Satisfactory results were generally obtained with the method consisting in taking samples of the two liquid layers in equilibrium and submitting them to chemical analysis; however, this method becomes delicate near the critical temperature. With this technique, Friedrich and waehlerts ob-

Jan 1, 1968

By R. W. Smashey, B. J. Piearcey

The structure, composition, and morphology of the carbide phases present in the nickel-base superalloy, Mar-M200, hare been determined and three carbide phases observed. The MC carbide is a solidification product, and the M23 Co and M6C carbides are both prod~icts of solid-state precipitation. The identity of each phase usas determined by both X-ray and electron-diffraction techn~ques. Compositions of all three carbides were studied using the electron beam micro-probe analyzer and by unalyszs of electrolytically extracted residues. Optical and electron microscopy were employed in order that the time/temperature -dependent behavior of the carbides might be observed. Supplementary studies were completed on thin foils and oriented single crystals to determine the mor-phology and orientation relationship of each phase with that of the matrix. MAR-M~OO* is a high-temperature, creep-resistant superalloy designed for use in the as-cast condition. The "as-cast" microstructure consists of a solid-solution matrix, referred to as gamma (y), which contains a general, coherent precipitate of the inter-metallic Ni3(A1,Ti) referred to as gamma prime (?). As a result of dendritic segregation during solidification, a degenerate, spherulitic ? -?' eutectic constituent is present at the grain boundaries and the in-terdendritic regions, which is nucleated by the y on the dendrite tips. A primary carbide phase, a solidification product, is also present at the grain boundaries and in the interdendritic areas, and an additional carbide appears at the grain boundaries as a fine discontinuous precipitate. The alloy is particularly susceptible to heat treatment. For example, the mechanical properties of the columnar grained mater- ial are substantially improved by solution heat treatment, followed by an intermediate temperature age. Metallographic examination of heat-treated material reveals, however, that exposure to elevated temperatures has a marked effect on the microstructure of the alloy; in particular, it is observed that precipitation of considerable amounts of various carbide phases occur. The following investigation was carried out to determine the morphology, composition, and behavior of the carbides in Mar-Ma00 as an aid to the determination of their effect on the mechanical properties and stability of the alloy. THE PRIMARY MC CARBIDE The MC carbide phase appears in the interdendritic interstices and the grain boundaries. In directionally solidified Mar-M200 the carbide appears as very small particles in the chilled region, Fig. l(a), whereas in material less affected by the chill, it becomes larger and develops a dendritic morphology, Fig. 1(b). Step polishing of metallographic specimens from this region shows that in directionally solidified material the individual carbide dendrites are connected in a dendritic network within the metallic interdendritic interstices, whereas in material from the chilled region and in conventional Mar-M200 they are discontinuous, isolated dendrites. No orientation relationship exists between the primary carbide and the matrix.

Jan 1, 1968

By Charles Bohdanowicz

Production of crude in 1937 decreased (Tables 1 and 5) by about 2 per cent, while gas production for that period increased by about 6 per cent after a slight decrease in 1936 (0.4 per cent).' As in preceding years, drilling operations were confined principally to extensions of old oil fields in the Jaslo district (fields 1 and 7) and to some extent to such extensions in the Stanislawbw district (field 27). Deepening of old wells to horizons reached more recently by new wells gave on the average better results per well than those attained by new wells (Table 3). Reserves of proved lands have increased some by new oil fields discovered, Targowiska (field 8) and Czarna (field 19) both of which, however, have only small production. The Daszawa gas field (field 25) has not been extended, but two new gas fields were located instead— Opary, distant 25 km. (151/2 miles) northwest of Daszawa, Balicze at 12 km. (7 1/4 miles) southeast of Daszawa, and Kalusz (TESP Company exploiting potassium salts) in the vicinity of the town of that name (field 33). Drilling upon the gas area near Tarnbw and Debica, while gas-bearing sandstone had been found at depths of from 300 to 512 meters (984 to 1680 ft.) (Zdziary No. 2) and at 220 m. (722 ft.) [pressure 11 atmospheres, flow 24 cu. m. per min. (847 cu. ft.)] (Przyborbw No. l), has not as yet ascertained horizons qualified for permanent exploitation. The exploring well near Kos6w remained for the last seven months at the depth of 1420 m. because of the collapse of rotary drilling pipe. Below the 300-m. level no gas sands have been encountered at this well. Gas Reserves In connection with the broad plan of developing industrially the sector of Poland lying between the Vistula and the San Rivers, and extending farther north as far as the city of Radom, there arose the necessity of a more accurate calculation of gas reserves for the fields of

Jan 1, 1938

By R. H. Schnitzel

Internal-friction peaks have been observed in tungsten single crystals at about 300° and 400°C. The characteristics of these peaks are similar to interstitial peaks observed in other bee metals; therefore, the origin of these peaks appears to he the Snoek mechanism. The interstitial responsible for the peak at about 300°C has not been identified. Carburizing increases the magnitude of the peak at about 400°C; consequently, it appears reasonable to suppose that the specific interstitial associated with this peak is carbon. The activation energies associated with the 300° and 400°Cpeaks are about 35,000 and 45,000 cal per mole, respectively. INTERNAL - friction peaks resulting from the stress-induced diffusion of interstitials (Snoek relaxation peaks) have been frequently observed in bee metals.1-5 Attempts to detect Snoek relaxation peaks in tungsten have, however, not been fruitful.' Failure to find Snoek peaks in sintered tungsten can perhaps be attributed to one or more of the following difficulties: a) the relatively low purity of the sintered tungsten; b) the lack of extensive metallurgical knowledge about tungsten-interstitial alloys, such as suitable interstitial dosing and quenching procedures; and c) the inconsistency of some of the interstitial analyses of tungsten, which reflects itself in one's inability to be sure of the nature of the specimens. This present investigation did not overcome all of these difficulties for successful tungsten internal-friction measurements. Some of these difficulties still persist and new difficulties were encountered during the course of this investigation. Nevertheless, the use of electron-beam tungsten single crystals having somewhat greater purity levels than sintered tungsten combined with appropriate carburizing and quenching procedures permitted a reasonable attempt to be made. As a consequence, internal-friction peaks were observed in these tungsten single crystals at about 300° and 400°C. These peaks were found to be unstable, since they annealed rapidly away during a sequence of internal-friction measurements. Hence, it was necessary to construct an apparatus having a faster heating rate to study some of the details of these peaks. From the behavior of these peaks as well as our knowledge of similar peaks in other bee metals, one can reasonably conclude that these peaks are caused by residual interstitial impurities within these crystals. Further investigation of these peaks after the application of various metallurgical treatments lent credence to this supposition. EXPERIMENTAL TECHNIQUE The internal friction of tungsten single crystals was measured using two different pieces of apparatus both of which are of essentially the same conventional design, namely the KE type of torsion pendulum. The important difference between these two types of apparatus was in the attainable heating rate and method of protection of the specimen from atmospheric contamination. The apparatus designated "number 1" was enclosed in a vacuum chamber which was heated by an externally mounted furnace. It had a slow rate of heating which was estimated to be about 4°C per min from room temperature to about 350°C and then about 1°C per min to 600°C. The internal friction of tantalum was measured with this apparatus and the established Snoek peaks were found.' These tantalum peaks in the temperature range from room temperature to 400° C served as a check for the apparatus. The apparatus designated "number 2" having a faster heating rate than number 1 was not elaborate. It consisted of a mounted nickel tube to which split heating elements were attached. Argon was used as the protective atmosphere. The measured heating rate was about 12° to 15°C per min whereas the cooling rate was somewhat slower at about 10° C per min because of the increased difficulty encountered in stabilizing the temperature. No surface oxidation of the specimen was noted after any test. This apparatus was also checked with the known peaks of tantalum.1 The preparation of the single-crystal specimens for internal-friction measurements consisted of centerless grinding the crystals from an approximate 0.200 in. diameter to 0.030 to 0.040 in. in diameter, and then electropolishing them to about 0.020 in. in diameter. Single crystals processed in this manner are designated as being in the virgin condition. Since the length of crystal varied from 3 to 9 in., the test frequency varied from about 1 to 2 cps. The frequencies of measurement, axial orientations, and chemical analyses for the various crystals are listed in Table I. The controlled addition of carbon into tungsten is a difficult problem. Attempts to find the critical conditions necessary for an equilibrium treatment were not fruitful. Therefore, a simple nonequi-librium method was used. The addition of carbon to these crystals consisted of appropriately combining three treatments—carburizing to achieve a case, annealing to partially dissolve the carbon into the

Jan 1, 1965

By B. Otto Pixler

Mud-analysis logging provides identification of the fluid content of formations drilled by the rotary method and permits the accurate correlation of oil and gas shows with the depth. Mud-analysis logging eliminates much coring and has an especially important application in drilling programs when coring is particularly hazardous or the electric log is difficult to interpret correctly. An appreciation of the factors that influence the results of the mud analysis, such as rate of penetration, mud properties, coring, and characteristics of reservoir rock as related to the "flushing effect," permits a better understanding of the mud-analysis log. Recent studies of the relationship of the two gas readings obtained by the gas-detector instrument have proved significant. The difference between the total combustible gas reading and the higher molecular weight gas reading indicates the presence of methane. With few exceptions, zones not showing an increase of methane probably can be condemned. Mud-analysis logging furnishes valuable information, which generally cannot be obtained by other methods. Introduction Logging by mud analysis of wells drilled with rotary tools is a direct method of locating oil-and-gas-bearing formations. The use of this method of logging has increased each year until now more than 20 field units are being used in 13 oil-producing states and in some foreign countries. Several papers1-9 have been published in the petroleum trade journals describing in detail the equipment and the application of mud-analysis logging. This paper will discuss briefly the method and review its application and some of the late developments. Method As the drilling of a well progresses, the drilling bit dislodges and disintegrates a cylindrical section of the formation. If oil or gas is contained in the pore spaces of the cylinder, some of the contents of these porous spaces will be entrained in the drilling fluid. In wall logging by mud analysis, the mud is continuously examined for oil and gas on its return to the surface, and the results are correlated back to the actual depth of the hole at the time the mud was clearing the eyes of the bit. The test for gas is made by diverting a portion of the circulating mud from the flow line to a separator or gas trap, where the mud is thoroughly mixed with air and a portion of the gas entrained in the mud is removed. A stream of air is drawn coun-tercurrent to the flow of mud in the gas trap, thus materially assisting the separation of the gas from the mud. The air-gas mixture is then drawn into a "hot-wire" gas-detector instrument where the percentage of the combustible gas is determined. The presence of oil in the formation drilled is detected by a physical examination of the drilling mud under ultraviolet light. A sample of the mud is treated to reduce the surface tension and gel strength, after which it is placed in a viewing box. This box is so constructed that all external light is excluded and so that the sample may be subjected selectively to either ultra-

Jan 1, 1946

By B. Otto Pixler

Mud-analysis logging provides identification of the fluid content of formations drilled by the rotary method and permits the accurate correlation of oil and gas shows with the depth. Mud-analysis logging eliminates much coring and has an especially important application in drilling programs when coring is particularly hazardous or the electric log is difficult to interpret correctly. An appreciation of the factors that influence the results of the mud analysis, such as rate of penetration, mud properties, coring, and characteristics of reservoir rock as related to the "flushing effect," permits a better understanding of the mud-analysis log. Recent studies of the relationship of the two gas readings obtained by the gas-detector instrument have proved significant. The difference between the total combustible gas reading and the higher molecular weight gas reading indicates the presence of methane. With few exceptions, zones not showing an increase of methane probably can be condemned. Mud-analysis logging furnishes valuable information, which generally cannot be obtained by other methods. Introduction Logging by mud analysis of wells drilled with rotary tools is a direct method of locating oil-and-gas-bearing formations. The use of this method of logging has increased each year until now more than 20 field units are being used in 13 oil-producing states and in some foreign countries. Several papers1-9 have been published in the petroleum trade journals describing in detail the equipment and the application of mud-analysis logging. This paper will discuss briefly the method and review its application and some of the late developments. Method As the drilling of a well progresses, the drilling bit dislodges and disintegrates a cylindrical section of the formation. If oil or gas is contained in the pore spaces of the cylinder, some of the contents of these porous spaces will be entrained in the drilling fluid. In wall logging by mud analysis, the mud is continuously examined for oil and gas on its return to the surface, and the results are correlated back to the actual depth of the hole at the time the mud was clearing the eyes of the bit. The test for gas is made by diverting a portion of the circulating mud from the flow line to a separator or gas trap, where the mud is thoroughly mixed with air and a portion of the gas entrained in the mud is removed. A stream of air is drawn coun-tercurrent to the flow of mud in the gas trap, thus materially assisting the separation of the gas from the mud. The air-gas mixture is then drawn into a "hot-wire" gas-detector instrument where the percentage of the combustible gas is determined. The presence of oil in the formation drilled is detected by a physical examination of the drilling mud under ultraviolet light. A sample of the mud is treated to reduce the surface tension and gel strength, after which it is placed in a viewing box. This box is so constructed that all external light is excluded and so that the sample may be subjected selectively to either ultra-

Jan 1, 1946

By P. E. Busby, C. Wells

FURTHER study of data used in determinations of 1—rates of diffusion of boron in austenite and 2—solubilities of boron in the a and phases of iron and steel' has provided an equation for the diffusion of boron in a iron. In brief, the previously published data were accumulated from the results of deboron-izing (and decarburizing) experiments carried out in the range of 700° to 1300°C. Diffusion coefficients (D?) for boron in austenite were calculated using the Grube solution of Fick's law. However, only solubility values were estimated from the discontinuous concentration-penetration curves, Fig. 1, which are characteristic of diffusion in two phases. Dr. Carl Wagner' has recently provided a solution for calculating D values from penetration curves of this type as follows: Cl1.1 —C8/C8- C11.1 = vp ? e ? erf (?) and D = ?/4?2 t where C11,12, C8, C11, and E have the values shown in Fig. 1. D is the diffusion coefficient, sq cm per sec; t is time of deboronizing anneal, see; and ? is a di-mensionless parameter. For a given diffusion experiment, the value of ? can be readily obtained by graphical solution from a plot of y vs the right-hand part of Eq. 1. D may then be evaluated from Eq. 2. The avplication of this solution to previously re-ported results, of which excerpts are given in Table I, permits the calculation of diffusion coefficients for boron in a iron. On the basis of these meager data, it is tentatively concluded that the diffusion of boron in a may be represented by the equation Da = 1011 e-92,900/RT where R is the gas constant, cal X 0C-1 X mol-1; and T is the absolute temperature, OK. Although the frequency factor, 106 sq cm per sec, is admittedly several orders of magnitude higher than expected, the value of Q, 62,000 cal per mol, appears reasonable and is, in fact, very similar to that for the self-diffusion of iron. It is pertinent to mention at this point that the value of Q obtained for the diffusion of boron in austenite by means of the Wagner solution is 19,000 cal per mol and is in excellent agreement with the value previously reported1 in the equation DT = 2xl0-3 e-21,000/RT [4] which was determined by the application of the Grube solution to other data. The fact that determined constants A and Q in the equation D? = A e-Q/RT were practically the same, independent of whether the Wagner or Grube solutions were used in determinations of D values, strengthened the authors' belief that the computed values of D (Table I) using the Wagner solution are reliable. The relative values in Eqs. 3 and 4 for the diffusion of boron in the a and ? phases, respectively, suggest that boron forms a substitutional solid solution in a iron and an interstitial solid solution in ? iron. The same tentative conclusion has been reached by McBride et al.3 on the basis of relative solubilities, atom diameter, and the size of the interstitial hole in a and ? iron. In connection with the data for test 14 listed in Table I, it is of interest to calculate the solubility of boron in a iron using the D value given by Eq. 3. As might be anticipated from the small movement of the interface in test 14, proper substitutions in Eqs. 2 and 1 give a low value, approximately 0.0004 pct B, at 850°C. Apparently at 835°C (test 13) it is possible to obtain 0.0018 pct B, and at 850°C only 0.0004 pct B into solution in the a phase before a second phase appears. These observations are consistent with the Fe-B constitution diagram proposed by McBride, Spretnak, and Speiser.3 References P. E. Busby, M. E. Warga, and C. Wells: Diffusion and Solubility of Boron in Iron and Steel. Trans. AIME (1953) 197, p. 1463; Journal of Metals (November 1953). 'W. Jost: Diffusion in Solids, Liquids, Gases. (1952) pp. 69-71. New York. Academic Press Inc. "C. C. McBride, J. W. Spretnak, and R. Speiser: A Study of the Fe-Fe2B System. Trans. ASM (1954) 46, p. 499.

Jan 1, 1955