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By R. D. Pehlke, J. F. Elliott

The equilibrium pressure of nitrogen gas over pure silicon metal and silicon nitride has been measured in the temperature range 1400° to 1700°C. From the experimental data, the standard free energies and enthalpies of formation of Si3N4(a) have been calculated as functions of temperature over the above temperature range. Utilizing data in the literature and the results of this investigation, the specific heat, molar enthalpy, molar entropy, standard enthalpy of fornation, and standard free energy of fornation are estimated for the temperature range 298° to 1400°C. THE high-temperature thermodynamic properties of many metallic nitrides are not well established at present. This is a serious deficiency because nitrogen and nitride-forming metals are important alloying additions to steels, and knowledge of the interaction between nitrogen and these elements is essential to a better understanding of the behavior of steels. Metallic nitrides also are used as refractory materials. Consequently, the investigation reported here was undertaken to provide more complete information on the standard entropy and free energy of formation of silicon nitride. The experimental technique provided a direct measurement of the equilibrium pressure of nitrogen gas in the range of 1413 to 1700°C for the reaction: 3 Si(1) + 2N2 (g) = Si3N4 (a) [ 1 ] and below 1413oC for the reaction: 3Si(c) + 2N2(g) = Si3N4(a) [2] APPARATUS The experimental system consisted of a crucible assembly, a reaction chamber, and a gas supply and vacuum system. The Crucible Assembly which contained the equilibration specimen and molybdenum radiation shields with a susceptor for induction heating is shown in Fig. 1. Two covered, high-purity alumina crucibles, one nested within the other, contained the susceptor, shields and specimen. Central openings in the upper shield and crucible covers permitted on optical pyrometer to be sighted into the central cavity of the specimen. The specimen itself was a 5/8 OD by 1-in.

Jan 1, 1960

By W. C. Phalen

The production of salt in the United States divides itself at the outset into two distinct classes…

Jan 1, 1915

By AIME AIME

BY COMBINING the sessions on reduction and refining of copper, lead and zinc it was possible to devote an entire day to nonferrous metallurgy. Four interesting papers were presented at the morning session and four more in the afternoon. In the discussion of papers on copper, F. R. Pyne acted as chairman, with H. M. Shepard as vice-chairman, whereas for those on lead and zinc, F. F. Colcord acted as chairman, with C. R. Hayward as vice-chairman. The paper by P. D. I. Honeyman on the smelting of raw concentrates in the reverberatory furnace was presented by Mr. Pyne and discussed by Messrs. Mazany and Hayward. The interesting paper by E. S. Bardwell, com- paring the use of various fuels in copper-refining furnaces at Great Fails, Mont., was presented by Mr. Shepard and discussed by Messrs. Boggs, Gronningsater and Hayward. That by R. G. Knickerhocker, describing the stationary basic copper converter at Messina, Transvaal, was presented by Mr. Pyne, together with a written discussion by c. R. Kuzell, of the United Verde Copper co. It was an interesting illustration of how well-known processes may sometimes be modified to fit into unusual conditions.

Jan 1, 1932

By G. E. Johnson

E. D. HYMAN*—How much sorting of scrap is done ? G. E. JOHNSON (author's reply)—We do practically no sorting. We charge "run of mine" scrap to the furnace. The unmeltables, mostly iron, are in such demand today that there is no difficulty in disposing of them. It may soon be desirable to sort out from the unmeltables as much of the brass as possible. J. J. BRUGMAN†—We have somewhat similar problems in the secondary aluminum business. What is your method of removing the unmelted material from the furnaces? Why have you such an apparently small space in which to charge your materials? Do you find that you have to seal that opening, or can you have it open and continuously charge at one end and pull out the other ? G. E. JOHNSON—Our means of melting scrap is efficient only to the extent that we use the waste heat from the vaporizing chamber to do the job. It is a batch process. We open the charge door and place the scrap on the hearth by hand shoveling. The door is then closed during the melting down period. After the melting is complete, the opposite door is opened and the unmeltables are raked out. The doors are approximately 3½ X 4½ ft and are not sealed during the process only closed. They are nominally tight. Some metal is oxidized in the process. We have visualized a means of conveying the materials through this melting unit with the metals that are melted trickling out during its travel. T. H. WELDON‡—Mr. Johnson, in line with the last question, is it necessary to seal the furnace between the melting down and the vaporizing unit, or have you got an inverted syphon in the bottom of the chamber? G. E. JOHNSON—That was one of the first things we encountered. We had to have a sealed opening, and it is a molten metal seal. You have indirectly asked me another question, which was: "Do you have to seal up the melting unit?" I would say we should exclude as much air as possible, although we are not too efficient in doing that. We allow the melting unit doors to be open when we charge and when we remove unmeltables. You can readily see that that would lead to the idea of having a controlled atmosphere in the melting unit, and I think this would do a more efficient job of melting the scrap. T. H. WELDON—How often do you charge the furnace? G. E. JOHNSON—We charge the melting unit, and rake out the unmeltables, about every hour. H. R. HANLEY*—Are any provisions made for controlling the rate of oxidation for the production of various size particles for certain characteristics of the zinc oxide product? G. E. JOHNSON—Yes, there are many. You are getting pretty much into the fine points of zinc oxide manufacture. Some of us still think we have something to learn about that. In general, this muffle furnace as I have described it to you produces a rounded particle of zinc oxide which is generally formed by a rapid oxidation of the zinc vapor, followed by rapid cooling. We have gone to the other extreme in some of our experiments. We have changed the furnace to produce a type of zinc oxide, such as we thought was peculiar to American process zinc oxide, by controlling the temperature at the point of oxidation and maintaining that temperature for a much longer period of time than we do when we make the rounded shape. There are other relationships that this furnace readily provides. One of the important factors is the ratio of air to zinc vapors. We can vary that by varying the air supply to the baghouse, or vary the rate at which we are vaporizing the zinc by the simple expedient of regulating the temperature over the carborundum arch. We have a number of variables that permit us to produce all of the grades of French process zinc oxide from lead-free up through the highest grades of seal oxides. There are many controls that we can apply to the operation. What I have said is but a brief condensation. K. MORGAN*—Can Mr. Johnson give us some idea of the fuel consumption of the furnace ? How much oil does he use per ton of zinc distilled? I am also interested to know what sort of heat transmission he gets through the arch? What is the thickness of the tiles used to construct the arch? Some time ago we built a small furnace for a different purpose, using a carborundum arch, and we found that the reflectivity of the molten zinc surface was so great we had to use a very high arch temperature. We found we made an improvement by having a layer of carbon on the surface of the zinc. Has Mr. Johnson had any experience on these points ? Does he make any sort of insolu-bles which he leaves in the furnace which he cannot tap out ? G. E. JOHNSON—I believe your first question was the fuel consumption. If I recall, somewhere in this paper there is a test that I quote. I believe we used 800 gal in a given period of time. Offhand I cannot translate that into tons of metal. I might also state that we have this understanding; that the carborundum arch, as the temperature becomes higher, becomes more efficient in heat transmission. As a matter of fact, I believe it is at about 2600°F or higher that the highest efficiency of heat transmission becomes available. We have calculations that I cannot quote from memory which indicate that the carborundum arch does a really very fine job for this type of furnace. Another point that we had considered was the fact that this furnace could be readily constructed so as to furnish an ideal source of heat for waste heat boilers. If a carborundum arch was used over the melting unit, we would have no zinc vapors in the gases at all— just clean combustion gases from which we would have removed some of the heat. L. P. DAVIDSON†— The insolubles

Jan 1, 1950

Francis Drake, Bulawayo, Rhodesia, So. Africa (communication to the Secretary *):—I should like to place on record some data in addition to those given by Mr. Canby in his paper. I regret that my notes have been destroyed so that I can give no accurate measurements of the water jacket that I am about to describe. This furnace mas erected in Cerro Gordo, Inyo county, Cal., early in 1875, and I think it quite possible that it was the first applied in lead smelting. It was made of plate iron and elliptic in shape, the inner dimensions being about 54 by 42 in. by 48 in. high. The distance between the inner and outer plates was about 6 in. Tuyere holes, one at the back and two on each side, about 12 in. in diameter, were made in this, and in these were placed cast-iron water tuyeres about 16 in. long, the diameter of the blast orifice at the point being about 3 in. The height from tuyeres to feed door was about 9 ft., but the top of the charge was kept about 5 ft. above the tuyeres. There was a space of about 12 in. between the jacket and the top brick-work. This brick-work was supported by a cast-iron plate resting on four cast-iron columns. At the beginning, the jacket was lined with air-dried radial bricks, made of crushed quartz and fire-clay, as it was thought that the jacket would not stand the heat on its bare plates. After a short time the practice was altered and no lining mas put in. The jacket was closed at the top and had a steam drum connected by two pipes at the back. This steam drum was connected to the boiler in which the steam was made for driving the Baker blower, the rock breaker and the pumps. The bottom of the jacket mas also connected to the boiler. The jacket was run under boiler pressure (80 Ib.) for some time, but eventually cracks developed in the inner plate between the tuyere holes,

Jan 1, 1913

By Walter J. Karplus, Otto J. M. Smith

The transient response of earth formations may be tlcter.171ined by means of four electrodes mounted coli-rienrly on n sonde. Exponentially decaying current pules are applied to one pair of electrodes and the re.rrrlting voltage transient at the other pair is recorded. It is shown by theoreticol analysis and verified by laboratory experiments that this arrangement readily yields the direct resistivity of the formation and provides valrrable additional information as well. INTRODUCTION Although electrical transients have been employed with moderate success in geophysical prospecting, their application to well logging has received virtually no attention in technical literature. In the conventional direct resistivity logging methods only the zero frequency impedance of the formation under study is measured, and no information is obtained regarding its reactive characteristics. Since the use of certain transients appears to offer some advantages in this respect, experiments were performed on a laboratory scale to investigate this possibility. This investigation was limited to a study of a four-electrode array where both the receiving and transmitting electrode pairs are mounted on a logging sonde, and decaying exponential pulses are applied to the transmitting electrodes. THEORY Given an electrode configuration as shown in Fig. I, located in a homogenous medium of resistivity p, if each electrode has an effective radius, r, which is small compared to the spacing, s and a, it is easy to show by integrating the volume resistivity that the input resistance, Rrw, of the transmitting electrodes is Rxw=p/2pr If a capacitor of capacity C, charged to a voltage Em, is suddenly connected to these electrodes, the resulting current, I(t), will then be The voltage transient, E(t), at the receiving electrodes may then be found by substracting the resulting potential at electrode Y from that appearing at electrode Z. and by inserting Eqs. 1 and 2 Integrating Eq. 4 with respect to tim

Jan 1, 1957

By W. W. Vaughn, R. H. Barnett, E. E. Wilson

Soon after the search for uranium ores on the Colorado Plateau began in earnest, thousands of feet of drill core ranging from 1 1/8 to 2 1/8 in. diam became available for study. Although significant advances had been made in the technique of quantitative gamma-ray borehole logging, instrumentation was in the development stage, and complete reliance could not be placed on gamma-ray logs alone to interpret quantitatively the meaning of radioactivity in a drillhole. A method that would be faster than chemical analysis and still give reproducible and reliable results for various drill core sizes was desirable to provide additional information on the enormous footage of drill core being accumulated. A solid phosphor scintillation drill core scanner was designed and constructed. Basically the instrument was developed to measure radiation from a drill core which would not be clearly recorded by a gamma-ray logger using a Geiger tube as the sensitive element. Such data would be beneficial in constructing isorad maps to delineate ore-bearing zones. A calibration in the range 0.01 to 0.1 pct eU.,O, was provided; above 0.1 pct eU3O8 gamma-ray logs were available and were being used to calculate grade and tonnage of ore reserves. The core scanner, however, has been used to estimate equivalent uranium content of ore-grade materials containing as much as 2.2 pct eU3O8 with an accuracy of ± 10 pct, the sample being in the form of a BX drill core. Actually, an apparent calibration of eU3O8 vs counts per unit time is a straight line with a slope that is a function of the sensitive element and the geometry of the counting assembly. A true calibration that will show the expected departure from a straight line is due principally to the random nature of the pulse from a radiation source and the nonlinearity of the electron circuitry. Design and Construction: Three methods of detecting radioactivity were considered and applied in developing the core scanner now in use: 1) the Geiger tube, 2) liquid scintillation phosphors, and 3) solid scintillation phosphors. The desired sensitivity and long-term drift characteristics needed for this operation could be attained only by using solid scintillation phosphors. All three methods are discussed. Before scintillation counters were common, nine beta-gamma sensitive Geiger tubes 7/8 in. diam by 12 in. long were used, arranged to surround the drill core with tube axes parallel to the axis of the core. This arrangement of Geiger tubes was en- closed in a lead shield 1 in. thick, and provision was made to slide a 6-ft length of drill core manually into the counting chamber, one foot at a time. A count for each segment was taken with a scaler while the core remained stationary. The equivalent uranium content of the different sections of drill core could then be estimated with the aid of a calibration curve of counts per unit time vs percent equivalent uranium (eU). In rare cases the effects of the radioactivity concentrated in small areas within the core introduced errors in the readings made with the Geiger tube arrangement owing to the geometry of the measurement. The variability of counting rate due to a localized concentration of radioactivity in a spot in the wall of a drill core is illustrated in Fig. 1. This effect and the inherent low efficiency of the Geiger tube were considered major disadvantages of this counting arrangement. When liquid scintillation phosphors became available the core scanner in Fig. 2 was constructed to make a more accurate measurement of the equivalent uranium content of a sample. This instrument contains about 4 liters of liquid phosphor in a stainless steel coaxial cylinder 1 ft long, with inner and outer walls 0.060 in. and 0.125 in. thick, respectively. Four end-window type photomulti-plier tube with cathodes of 2 in. diam, immersed in the solution at right angles to the axis of the core, were used to observe light flashes in the phosphor. The liquid phosphor offered equal sensitivity to radiation originating at any point in the enclosure and represented geometrically the optimum in design. However, providing a semi-permanent leak-proof seal between the glass envelope of the phototube and the metal walls of the container proved to be a serious problem in constructing the equipment. The most effective seals were especially machined O-rings from sections of large tygon tubing. The tygon took a permanent set owing to cold flow characteristics and in most cases sealed completely. The light absorption characteristics of the liquid phosphor changed gradually with time, and after one month the counting rate had decreased to half the original value. The most sensitive liquid phosphor tested proved to be a solution containing 4 g of 2.5-diphenyloxazole and 0.01 g of 2-(1-naphthy1)-5-phenyloxazole per liter of toluene. With fresh solution in the chamber and with all photomultiplier tubes operating in parallel, the counting rate contributed by any one of the four photomultiplier tubes was about 85 pct of the counting rate from a single tube operated individually. From these observations it was concluded that owing to coincident loss and light attenuation within the liquid phosphor, the apparent sensitivity could not have been materially increased by additional phototubes. However, this approach to core

Jan 1, 1960

By Gorr W. W., Wyche E. H, R. Smith

The combination of high strength and corrosion resistance of cold-worked 18 Cr, 8 Ni steel has been advantageously utilized for some time, particularly in aircraft and rail car structures. There are, however, certain limitations on the use of such materials because the high strengths can be obtained only by cold-working, limiting the available products to sheets, strip, wire and tubes. The authors sought to overcome these limitations by resorting to precipitation-hardening, which has been used so successfully in nonferrous metallurgy but only to a limited extent in iron-base alloys. Accomplishment of this objective not only overcame the limitations, but also effected certain improvements in mechanical and other properties. This paper is an account of the development by Carnegie-Illinois Steel Corporation of a precipitation-hardening 18-8 stainless steel (called Stainless W‡ and tentatively identified as type 322). A description is given of its composition and metallurgical characteristics, heat-treatment, physical and mechanical properties and corrosion resistance. Development of the New Steel For a considerable length of time the authors were unable to determine the mechanism of the precipitation-hardening process that had been noted by Ffield18,19 in 18-8 Ti or 18-8 Cb after cold-working and reheating to moderately elevated temperatures. All known variables were exhaustively studied, but with little success. However, results began to indicate that chemical composition was the most important variable, particularly the ratio of austenite-forming to ferrite-forming elements. The investigators then focused their attention upon the composition, and, in particular, upon the element titanium and its mode of alloying in the presence of other elements. A heat was obtained that could not be brought to the softness level of annealed 18-8. The response to cold-straining and aging* was very marked by previous standards, and, more important, cold-straining was found to be entirely unnecessary to produce the precipitation-hardening effect. The chemical composition of this heat was: C, 0.06 per cent; Mn, 0.54; P, 0.016; S, 0.016; Si, 0.58; Ni, 7.28; Cr, 17.60; Ti, 0.90; Al, 0.17. For some time the development work, particularly on composition, was carried

Jan 1, 1947

By Gorr W. W., R. Smith, Wyche E. H

The combination of high strength and corrosion resistance of cold-worked 18 Cr, 8 Ni steel has been advantageously utilized for some time, particularly in aircraft and rail car structures. There are, however, certain limitations on the use of such materials because the high strengths can be obtained only by cold-working, limiting the available products to sheets, strip, wire and tubes. The authors sought to overcome these limitations by resorting to precipitation-hardening, which has been used so successfully in nonferrous metallurgy but only to a limited extent in iron-base alloys. Accomplishment of this objective not only overcame the limitations, but also effected certain improvements in mechanical and other properties. This paper is an account of the development by Carnegie-Illinois Steel Corporation of a precipitation-hardening 18-8 stainless steel (called Stainless W‡ and tentatively identified as type 322). A description is given of its composition and metallurgical characteristics, heat-treatment, physical and mechanical properties and corrosion resistance. Development of the New Steel For a considerable length of time the authors were unable to determine the mechanism of the precipitation-hardening process that had been noted by Ffield18,19 in 18-8 Ti or 18-8 Cb after cold-working and reheating to moderately elevated temperatures. All known variables were exhaustively studied, but with little success. However, results began to indicate that chemical composition was the most important variable, particularly the ratio of austenite-forming to ferrite-forming elements. The investigators then focused their attention upon the composition, and, in particular, upon the element titanium and its mode of alloying in the presence of other elements. A heat was obtained that could not be brought to the softness level of annealed 18-8. The response to cold-straining and aging* was very marked by previous standards, and, more important, cold-straining was found to be entirely unnecessary to produce the precipitation-hardening effect. The chemical composition of this heat was: C, 0.06 per cent; Mn, 0.54; P, 0.016; S, 0.016; Si, 0.58; Ni, 7.28; Cr, 17.60; Ti, 0.90; Al, 0.17. For some time the development work, particularly on composition, was carried

Jan 1, 1947

By W. L. Austin

At the Steptoe metallurgical plant, where ore of the Nevada Consolidated Copper Co. is beneficiated, a small copper-leaching annex has been in operation treating flue dust from roasting-furnace dust chambers, together with a siliceous oxidized ore. This leaching plant was designed to obviate smelting low-grade siliceous flue dust, which interfered with the operation of the reverberatories by forming a blanket on the charge. The major portion of the copper content of the flue dust accumulating in the upper chambers of the roaster flue, and at the stack, is water soluble, and also contains much free sulphuric acid and soluble sulphates. It was found that sufficient acid could be obtained by mixing this material with water to provide a lixiviant for leaching the siliceous copper ore mentioned. This was the sole source of the lixiviant used in the operation to be described. An analysis of the flue dust showed it to be composed as follows : Per Cent. Copper.............................................. 3.00 siO2................................................. 23.41 Fe................................................... 4.08 CaO + MgO......................................... 2.72 Al203................................................ 0.07 Free H2S04........................................... 19.94 SO3 combined as sulphate.............................. 25.10 H2O combined with the sulphates....................... 10.67 0................................................... 2.50 Total................................... 97.49 Copper soluble in dilute H2SO4.......................... 2.56 The oxidized ore, locally known as carbonate, has the following composition:

Jan 1, 1915

By W. M. Bertholf

To establish the minimum or break-even efficiency of a preparation plant it is necessary to determine the ratio of production costs per ton of run-of-mine coal to sale price per ton of clean coal. This ratio is then divided by the percentage of plant recovery. Assume, for example, that washability data indicate that 80 pct of the run-of-mine coal may be recovered as clean coal selling for $5.50 per ton. If the same plant incurs $4.00 per ton mining costs and $0.25 per ton preparation costs, the cost to sale price ratio would be 4.25/5.50, or 77.3 pct. Since the plant is capable of recovering 80 pct of the run-of-mine coal the minimum plant efficiency would be 77.3/80, or 96.6 pct. If the plant efficiency were increased to 100 pct the limit on preparation costs would be increased to $0.40. Therefore, the washing operation must be accomplished at a cost of $0.25 to $0.40 per ton and the efficiency must be 96.6 pct or higher. By plotting a curve of efficiency vs preparation costs and taking into consideration the plant cost, feed rate, operating costs, and yields of the various flowsheets it is possible to select a financially sound process. Table I classifies preparation processes according to their nature of separation. It must be remembered that what is thought to be ideal does not always prove practical under actual operation. An outstanding example is the work done on the plunger-type jig. It was determined by the law of equivalence that this unit could treat satisfactorily only sizes differing by no more than a ratio of 2. Yet these same plunger-type jigs are successfully treating sizes considerably greater than this ratio.

Jan 12, 1957

By G. D. Gemmell

Effects of solid-sdutidn alloying with titanium, molybdenum, and tungsten at concentrations up to 10 pct on the strength of pure columbium at elevated temperatures (mainly 2000°F) have been investigated by means of creep-rupture, hot-tensile, and hot-hardness testing and recrystallization studies. ThIS paper presents some results from the initial part of a study of the effects of alloying on the high-temperature strength properties of columbium. The elevated-temperature strength characteristics of pure columbium were first studied. Binary alloys of columbium with titanium, molybdenum, and tungsten containing 1, 5, and 10 pct of the solute elements were chosen on the basis of their high melting points, their known solid solubility in columbium, and results of separate oxidation-resistance studies of columbium alloys. EXPERIMENTAL PROCEDURE All the materials used were of highest purity. A typical analysis of the columbium is shown in Table I. Compositions of the alloys are also given in Table I. To evaluate the strength properties of pure co-lumbium and the alloys at elevated temperatures, creep-rupture, hot-tensile, and hot-hardness testing was done on recrystallized material. To prepare the pure metal and the alloys for these tests, 1- 1b buttons were made in a water-cooled copper crucible, inert atmosphere, tungsten arc furnace. Tapered ingots, 3 in. long, were made from these buttons by a skull-casting technique and these were machined to 1/2 in. diam, swaged to 50 pct reduction (pure columbium at room temperature, alloys at lowest temperature possible without cracking, generally in range 1100" to 1800°F) and heated in vacuum (lo-' mm Hg) for 16 hr at 2550°F for re-crystallization and homogenization. The resulting grain diameter was 0.1 to 0.3 mm. The 10 pct Mo alloy casting was not successfully swaged at temperatures up to 1800°F without cracking and was not included in the test program. Creep-rupture testing was done at constant load in vacuum on cylindrical specimens of 0.16 in. diam, using Instron capsules. The pressure at test temperatures was less than 10-1 mm Hg. Hardneas readings taken on the test specimen before and after testing were used as a check on possible gaseous contamination. Hot tensile tests in vacuum on cylindrical specimens of 0.125 in. diam were also made with Instron equipment at a strain rate of 0.067 min.-l. Hot-hardness measurements were taken with a unit constructed at the Du Pont Experimental Station. The test piece, supported on an alumina anvil, and the molybdenum indenter shaft with sapphire tip is heated in a platinum-wound furnace. The load applied to the pyramid indenter is measured by strain gages attached to a proving ring located outside the hot zone. In the measurements reported here the load was I kg. The tester operates in a vacuum of about 10"5 mm Hg and is capable of temperatures up to 1400°C.

Jan 1, 1960

By W. N. Lacey, R. H. Olds, B. H. Sage

The volumetric behavior of five mixtures of black oil and natural gas and of two mixtures of condensate and natural gas from a field in the San Joaquin Valley was experimentally established. This work was carried out at roo°, I9o° and 250°F in the pressure interval between 400 and 5000 psi. The viscosity of the liquid phase of four mixtures of black oil and natural gas was experimentally measured in the above-indicated temperature and pressure intervals. The effect of methane upon the precipitation of bitumen from the black oil was studied at 230°F. Introduction The solution of a number of the economical and technological problems which arise in connection with petroleum production is dependent upon the availability of the necessary quantitative information covering the materials involved. This requires data concerning physical properties of naturally occurring hydrocarbon mixtures at the pressures and temperatures characteristic of underground petroleum reservoirs. The experimental determination of the desired data for each situation encountered is relatively time-consuming. However, it is considered to yield results sufficiently more reliable than those obtained from correlations to justify the effort. For these reasons there was undertaken a laboratory investigation of the viscosity of the liquid phase and the volu- metric and phase behavior of mixtures of oil and gas samples obtained from wells in a field located in the San Joaquin Valley. Terminology The nomenclature of petroleum engineering is not at present entirely standardized. Many commonly used technical terms are not everywhere given the same meanings. For the purposes of this paper the following definitions will be adopted: Black oil refers to the dark-colored, hydrocarbon liquid obtained when the producing horizon of the well lies partly in the condensed hydrocarbon phase of the reservoir. Condensate is the term applied to the relatively volatile, pale yellow or amber-colored hydrocarbon liquid that is often obtained from the surface separator system when the producing horizon of the well lies in the gas cap of the reservoir. The gas obtained from the surface separator system is called natural gas regardless of whether the well is producing black oil or condensate. As might be expected from the multi-component character of naturally occurring hydrocarbon materials, the compositions of black oil, condensate and natural gas are subject to considerable variation depending upon the temperatures and pressures prevailing in the surface separator system as well as upon the overall composition of the material produced from the reservoir. In order to obtain samples capable of reproducing the total hydrocarbon material produced by the well, all oil and gas mixtures used in this investigation were com-

Jan 1, 1949

By D. A. Koss, R. O. Gordon

Changes in the ultrasonic attenuation in steel specimens have been observed during tensile tests. Samples of AISI 1020, 1045, and 1095 steel quenched and tempered to a spheroidized condition have been used. Both attenuation and microstrain measurements fail to reveal preyield dislocation motion in the as-tempered specimens. Upon reapplication of the load to samples in the strain-aged condition there is a large preyield attenuation increase but no observable micvostrain up to 90 pct of the flow stress. These and other observed changes can be related to changes in the free disloca-tion density and the average dislocation segment length. The results show that the increase inflow stress in the strain-aged condition is caused by increased fric-tional stresses rather than by dislocation pinning. Strain aging is found to proceed through three distinct stages. The second of these follows the t2,3 law and is characterized by an activation energy of 20 kcal per mole. RECENT years have seen substantial progress in the understanding of the sharp yield-point phenomenon in metals; the influence of solute atom pinning of dislocations, of dislocation multiplication, and of the stress dependence of dislocation velocity on the stress-strain curve has been investigated. Evaluation of the relative importance of these factors in the various metals and alloys is not complete, however, because observation of the stress-strain curve alone is not sufficient to determine the yield mechanism. In the experimental study of the sharp yield point it would be desirable to be able to directly observe the dislocations in a bulk specimen. Ideally, the observations should be made during deformation because of the rapidity of recovery processes in lightly strained metals. While direct observation of dislocations under these conditions is not possible, certain physical properties sensitive to the dislocation structure can be observed while a test specimen is undergoing deformation. Of these properties, one of the most useful is the ultrasonic attenuation. The total observed attenuation, a, is due to a number of causes: acoustic diffraction, scattering by inhomogeneities in the structure, heat flow, magnetostriction, and dislocation damping. Satisfactory measurements of the absolute a are difficult to make because all of these factors cannot be evaluated in any given specimen, but changes in a due to changes in the dislocation contribution alone can be reliably observed by appropriate technique. Because dislocation damping is sensitive to small concentrations of long, free dislocation segments, observation of acoustic attenuation due to dislocations is particularly useful in the study of the early stages of plastic deformation. In the experiments to be described, acoustic-attenuation measurements have been made on steel samples as these were pulled through their yield in tension. While many details of dislocation-damping phenomena in the bee metals remain obscure, the main characteristics of this type of internal friction are established. At low strain amplitudes and at frequencies well below that of dislocation resonance (the conditions of these experiments) the dislocation contribution to a is given by1 where A is the density of freely oscillating dislocation segments, L is the average segment length, B is the damping constant for a moving dislocation, w is the frequency, O is an orientation factor, C is the dislocation line tension, and t is a numerical factor relating average segment length to the distribution of lengths. Because of its fourth-power dependence on L, a is highly sensitive to changes in dislocation free segment length such as might arise from unpinning, recovery, jog formation, or dislocation intersection. The above equation is not valid near the resonant frequency of dislocations, but the segment length in steel is believed to be much too short to cause over-damped resonance near 10 Mc; this will be discussed later. In the present experiments plastic-strain measurements with a sensitivity of 2 x 10-5 were also made during the early stages of loading in order to detect preyield strain. The general plan of the experiments is to observe

Jan 1, 1967

By Charles L. Mantell, James E. Hoffmann

Mechanical inclusion, electrophoretic deposition, and adsorption were studied as mechanisms for code-position of aluminas present in copper-plating electrolytes as an insoluble disperse phase. Mechanical inclusion was not a significant factor. That codeposi-tzon of aluminas by an electrophoretic mechanism was unlikely was substantiated by measurements of the potential of the aluminas. The alumina content of the deposits was studied as a function of the pH of the bath. These tests in conjunction with sedimentation studies demonstrated the absence of an isoelectric point for the alutninas over the pH range examined. Thiourea in the electrolyte (a substance known to be adsorbed on a copper cathode during electrodeposition) affected the amount of alumina in the electrodeposit. However, no adsorption of thiourea on aluminas in aqueous dispersions was detected. If it were possible to produce a dispersion-hardened alloy of copper and alumina by electrodeposition, an alloy possessing both strength and high conductivity at elevated temperatures might be anticipated. Investigation of the mechanism of codeposition of aluminas with copper was undertaken with the hope that knowledge of the mechanism would aid in the development of such an alloy. The word "codeposit" here does not necessarily imply an electrolytic phenomenon but rather that the materials codepositing, the various aluminas, are transported to and embedded in the electrodeposited copper by some means. Mechanical inclusion in electrodeposition implies a mechanism of codeposition which is wholly mechanical in nature; the only forces acting on a particle are gravity and contact forces. Such a particle is presumed to be electrically inert and incapable of any electrical interaction with electrodes in an electrolytic plating bath. Processes for matrices containing a codeposited phase by electrodeposition from a bath containing a disperse insoluble phase frequently state that code-position is caused by mechanical inclusion.10,2,12 If settling, i.e., gravity, be the controlling mechanism for codeposition of aluminas, then assumptions may be made that 1) the content of alumina in the electrodeposit should be enhanced by increasing the particle size, 2) the geometry of the system, that is, the disposition of the cathode surfaces relative to the di- rection of the falling particles, should affect the alumina content of the electrodeposit, 3) in geometrically identical systems the chemical composition of the electrolyte employed should exercise no effect on the alumina content of the deposit, that is, the alumina content should be the same in all cathode deposits irrespective of bath composition. A bent cathode19 evaluates the clarity of filter effluent in electroplating baths by comparing the roughness of the deposit on the vertical surface with that on the horizontal surface. Two difficulties are inherent in this technique: 1) the current density on the horizontal portion of the cathode would be substantially greater than that on the vertical surface; 2) should the deposit obtained be rough, projections on the vertical face could act as horizontal planes and vitiate the relationship between the vertical and horizontal surfaces. Bath composition should have no substantial effect on the alumina content of the deposit. Two different electrolytic baths were employed. They possessed variant specific conductances and substantially different pH ranges. The experimental tanks were rectangular Pyrex battery jars 6 in. wide by 3 1/4 in. long by 9 3/4 in. deep. The cathodes were stainless steel 316 sheet of 0.030 in. thickness, cut to 7.5 by 1.75 in. and bent at right angles to form an L-shaped cathode whose horizontal surfaces measured 1.75 by 3.0 in. All edges and vertical surfaces were masked with Scotch Elec-troplaters Tape No. 470. The anodes were electrolytic cathode copper 9 in. high by 2.25 in. wide by 0.5 in. thick. To eliminate inordinately high current densities on the projecting edge of the cathode, the anode was masked 1 in. above and below the projected line of intersection of the cathode with the anode. The exposed area of the anode was equal to that of the cathode, providing both with equal average current densities. The agitator in the cell was of Pyrex glass and positioned so its center line was equidistant from cathode and anode, and a plane passed horizontally through the center of the blade would be located equidistant from the bottom of the cathode and the bottom of the deposition tank. The assembled apparatus is depicted in Fig. 1. Hatched areas on anode and cathode represent the area of the electrodes wrapped with electroplaters tape. MATERIALS The chemicals were copper sulfate—CuSO4 • 5H2O— technical powder (Fisher Scientific Co.). Spectro-graphic analysis showed substantial freedom from antimony, arsenic, and iron. Traces of nickel were present.

Jan 1, 1967

By W. E. Quist, R. Taggart, D. H. Polonis, C. J. van der Wekken

An intermediate compound that has been identified as Niab is observed to form as a decomposition product from supersaturaled Ni-Nb solid solutions during aging at temperatures between approximately 300" and 500°C. On the basis of data from electron microscopy and selected-area diffraction, the structure of this compound has been determined as fct with a = b - 3a0 and c = a, wlzere a,, is the lattice parameter of the parent solid solution. The compound consists of close-packed layers with triangular ordering, where the niobiutrl atoms are separated by two nickel atoms ([long- close?-packed directions. A nine layer stacking sequence is required to describe the proposed structure. STUDIES of the Ni-Nb binary system have been limited primarily to phase diagram determinations,'-4 investigations of high-temperature equilibrium phases,5"1 and the determination of the influence of deformation on the structure of the equilibrium compound.8 The nickel-rich portion of the binary system is reported to be of the simple eutectic type in which the maximum solubility of 12.7 at. pct Nb occurs at 1282"c.' The two-phase field below the eutectic temperature is bounded by the a fcc solid solution and an orthorhombic Ni3Nb compound. No metastable phases have been reported in previous investigations. In transformation studies of certain nickel-base commercial alloys that contain niobium, two ordered metastable compounds containing niobium have been shown to precipitate from the solid solution, both of which have been identified as y' and have the composition NisNb or Ni,Nb. One compound has been reported to have the bct DOz2 type Al3Ti structure" and the other the cubic LI2 type Cu3Au structure.9,11 In the present work on Ni-Nb binary alloys a metastable y' compound has not been detected after conventional quenching and aging treatments. An anomalous behavior was noted in electrical resistivity measurements. in alloys containing between 7 to 12 at. pct Nb when aging treatments were performed below 500°C after fast quenching from 1250°C. Transmission electron microscopy has shown that this behavior is caused by the formation of a low-temperature precipitate of unreported structure type and composition. EXPERIMENTAL METHODS Several Ni-Nb alloys, containing up to 11.5 at. pct Nb. were prepared by either levitation melting and casting in copper molds or by induction melting in alumina crucibles; both techniques employed purified helium gas as a protective atmosphere. The purity of the nickel and niobium used to make the alloys was 99.98 wt pct Ni and 99.9 wt pct Nb. The composition and homogeneity of the alloys were checked by weight measurements and by electron microprobe analysis. The induction-melted alloys were homogenized for 100 hr at 1100°C. The resistivity specimens were prepared from rods swaged to 2.5 mm and the electron microscopy specimens were cut from sheet that was rolled to 0.4 mm and thinned using a modified Bollmann technique." The elevated-temperature solution treatments were carried out in a purified helium atmosphere followed by direct quenching into a 10 pct NaCl solution at 23°C. Additional protection against oxidation of the samples during solution treatment was accomplished by using tantalum foil as a "getter" in the furnace. The specimens were aged at various temperatures in salt baths controlled to +2oC. A Leeds and Northrup K5 potentiometer was used to make electrical resistivity measurements on specimens immersed in liquid nitrogen. Electron microscopy and diffraction studies were carried out with JEM-7 and Philips EM-200 microscopes operating at 100 kv. RESULTS AND DISCUSSION Ni-Nb alloys containing between 7 and 11.5 at. pct Nb that have been solution-treated in the range 1220" to 1280°C and quenched to 23°C undergo a precipitation reaction when aged in the temperature range 300" to 500°C. Precipitation was detected by selected-area electron diffraction after aging a specimen for as little as 30 sec at 350°C) whereas the reaction was well-advanced after aging for 150 hr at 475°C. Electrical resistivity measurements were used to monitor the progress of the precipitation reaction. In the present experiments the nucleation process for precipitation required a high solution temperature and a rapid quench into brine. The presence of aluminum, iron? and carbon in amounts totaling less than 1 wt pct was found by electron diffraction to completely suppress the formation of the low-temperature precipitate that has been detected in the binary alloy. Electron diffraction techniques were used to determine the structure of the precipitates that formed during the decomposition of the Ni-Nb supersaturated solid solutions. Figs. l(a) through l(d) show electron diffraction patterns oriented to the [loo], [110], [lll], and [I031 zone axes of the matrix. Areas of reciprocal space between these sections were investigated by slowly varying the orientations of the crystal under study; this procedure revealed no reflections other than those depicted in Fig. 1. The presence of super-lattice reflections at points coincident with the matrix reflections was confirmed by the examination of an almost completely transformed structure. On the basis of the accumulated diffraction data, the reciprocal lat-

Jan 1, 1970

By J. A. Clum, R. W. Heins, T. D. Tiemann

The use of Na-montmorillonite clay hinders (Western Bentonite) in the pelletizing of iron ore concentrates is well established as is the idea that alternative binders must be found. 1-6 This note summarizes work done7 in evaluating a Wisconsin montmorillonite clay binder. The clay occurs in irregualr beds overlying the Prairie du Chien Dolomite and the St. Peters Sandstone near Hersey, St. Croix County. The raw Wisconsin clay contained 65% quartz and 35% clay minerals. The Na20to CaO ratio was 0.234. Suspension viscosity tests of the raw clay gave results only slightly better than water alone, even after treatment with activator materials. Sedimentation treatment reduced the quartz in the decantate to 5% after 240 min (four hours). Twenty minutes of sedimentation produced a decantate with 27.5% quartz which was found as effective as the 5% quartz decantate in pelletizing behavior. The 20 min decantate was used in subsequent tests. The decantate was filtered and dried at 110°(230°F). The minus 200 mesh portion of this was added directly to the magnetite concentrate. Pellets were made in a laboratory sized disc pelletizer from pastes consisting of ore concentrate, balling water (9%) and binder (clay, or clay + resins, or resins). The pastes were premixed in a Waring blender. The binders were: (1) 1% of a commercially used Western Bentonite; (2) 1 % or 3% of the Wisconsin clay (raw, or 20 min decantate); (3) 20 min decantate washed with activator solutions, (to exchange Na for Ca in the clay); (4) decantate with activator added in the balling water; (5) decantate with organic resins; (6) organic resins. Measurements of the 0.46 m (18 in.) Green Drop Number, the Dry Strength and the Fired Strength (fired at 1260°C (2300°F) for 30 min) were made. The dry and fired compressive strengths were determined on an Instron testing machine using a C-load cell and a F-load cell, respectively. The cross-head speed was 0.004 m/sec (0.1 in./min) for both. The results of each measurement were averaged for 15 pellets. A summary of those results is presented in [Table 1]. More detailed results and procedures are presented in another report.7 In addition to the effects on pellet strength due to various binders the effect of varying magnetite concentrate characteristics is noted in [Table l]. There, a few comparative data are shown for Cornwall, PA Magnetite, which has a generally liner particle size than the Black River Falls magnetite which was used for most of the tests.

Jan 1, 1979

By Orville R. Lyons, A. C. Richardson

During the past few years there has been a growing demand by coal operators for detailed information about the performance characteristics of the various dryers now being manufactured, preferably in such a form that the information could be used to determine the type of dryer best suited to a particular drying problem. A few operators have been desirous of going even further, because they are of the opinion that present-day dryers are not properly designed and that fundamental studies of dryer design should be undertaken. This growing demand for a method of dryer evaluation and the indicated need for fundamental research resulted in the sponsorship by Bituminous Coal Research, Inc. of a project at Battelle Memorial Institute to investigate the thermal drying of coal. In investigating this problem, the most feasible method of attack appeared to be a survey of active operations to determine the present status of the thermal drying of coal. Data were obtained, usually by actual plant tests with the cooperation of the various preparation engineers and their staffs, for 9 screen-type dryers, 8 rotary-type dryers, 3 continuous-pallet-type dryers, 2 flash-type dryers, I tray-type dryer, and I cascade-type dryer. The testing program provided: (I) data for 24 coal-drying operations, (2) information about the inherent characteristics of the coals dried, (3) information about the previous treatment that the coal had received, and (4) information about operating costs. The data obtained through the dryer survey and relationships determined from the data make it evident that all of the types of dryers included in the survey can be operated with the same degree of effectiveness if each type of dryer is used to dry the sizes of coal for which it is best suited. It should be noted that it is usually undesirable and often impossible to dry different sizes of coal in one type of dryer. By use of the data in the report, any prospective dryer user, having determined the surface moisture percentage and screen-size analysis of the coal to be dried, the tons of water to be removed per hour, and the final surface moisture percentage desired, should be able to determine with a fair degree of accuracy: (I) the difficulty of the drying problem, (2) the approximate cost of drying, (3) the required dryer inlet gas temperature and volume and exhaust gas temperature and volume, (4) the type of dryer to use, and (5) the size of dryer required. The method of testing the dryers and determining the difficulty of drying can be used by operators already having dryers to check the performance of their particular dryer and determine whether they are operating effectively. Considerably more information was obtained from the survey of thermal drying than was anticipated when the survey was first considered. However, a great deal of work still remains to be done in the field

Jan 1, 1949

By John Bonar

A switch to refractory-type slurry pump linings has significantly reduced maintenance costs arising from liner failure at a Missouri lead mill. The pumps routinely handle a slurry consisting of 79 to 81% solids with occasional tramp iron, and are subjected to intense abrasion which previously wore out rubber liners in anywhere from three days to two months. Average liner life at the 1.5-million-t/y (1.6-million-stpy) operation was 30 days. Experimentation with mild steel liners and even manganese steel liners failed to extend liner life beyond two months.

Jan 3, 1978

By R. W. Brauchli

The author has made a statistical analysis of the relations between recovery and length of cores, diameters of cores and of drill pipe, and cost of coring under different contractual conditions. The data are presented in tabular form. The length of the core appears to play a minor part in the percentage recovered, with a tendency to lower percentages with increased core length; approximately 50 per cent of the length cored is normally recovered if the cores are more than 2 in. in diameter. The diarneter of the core has a more pronounced influence on the recovery; 1 3/8-in. cores average 29.1 per cent, 2 1/8 -in. core 53.4 per cent and 3 1/8-in. cores with 6 5/8-in. drill pipe 68.5 per cent. Where 31/8-in cores were taken with smaller diameter drill pipe, i. e., 4 1/2 - in. drill pipe in 8 1/4-in. hole, the recovery dropped to 49.8 per cent, indicating that the more rigid drill pipe favors good core recovery, a conclusion also borne out by the results obtained in using large drill pipe for smaller diame-ter cores. Surprisingly good recoveries were obtained from both the Johnson and Simpson sands; shale, limestone and dolomite each gave less then average recoveries. No serious fishing jobs resulted from coring operations. Attention is called to the need of a core drill which will make it possible to drill a full-sized hole while coring, and thus reduce the cost of cores. Data pertaining to core drilling should be consistently recorded, such as, diameter of drill pipe and collar, diameter of core, recovery, size of cutter heads, type of core-barrel, coring time, speeds of rotation and of pumps, weight on core-barrel, etc.

Jan 1, 1933