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By J. M. Oblak, R. F. Hehemann, R. H. Goodenow

STUDIES of surface relief and growth kinetics have lead to the concept that widmanstatten ferrite along with upper and lower bainite constitute a continuous series of decomposition products.1-4 Current models4 propose that these products form as plates with a coherent or semicoherent leading edge which propagates at a rate controlled by diffusion of carbon into the surrounding austenite. There are, however, important crystallographic and morphological differences between these products—particularly between upper and lower bainite. For example, upper bainite appears to exhibit a (11lIy orientation habit, whereas lower bainite develops with a more irrational habit near {2251y.5-7 Many of the morphological features of these decomposition products are not yet well-documented. Recent studiess have demonstrated that low-carbon martensites form as sheets of closely spaced needles on {lllly planes while higher-carbon martensites form as plates with {225}? or other orientation habits. The similarity in the crystallography of these two modifications of martensite with upper and lower bainite is striking. Therefore, a study of the morphology of bainite in a series of hypoeutec-toid alloy steels has been initiated to explore these relationships further. The question of immediate interest is whether upper and lower bainite form as plates or needles. A two-surface (approximately perpendicular) metallographic method was employed to study the morphology of bainite in a variety of low and medium alloy steels. Compositions of these steels have been reported elewhere. The behavior of 4340 and 4370 was typical and will be described here. Austenitizing treatments involved 20 min at 2350°F for 4340 and at 2000°F for 4370. Isothermal transformation was conducted in molten-salt baths. Upper bainite was produced at 925°F in the 4340 steel and lower bainite at 575°F in 4370 with transformation times adjusted to produce 10 to 15 pct of the decomposition product. Many of the morphological features of upper bainite have been catalogued in the recent literature.'' The two principal variants observed in the present investigation are illustrated in Fig. l(a). One form appears as long, thin plates or needles and the other as small, frequently irregularly shaped particles. Both variants may occur as isolated forms but more frequently appear in groups as demonstrated in Fig. l(a). Two-surface analysis reveals that these two variants constitute different sections through a single morphological form. To demonstrate this, a number of sections perpendicular to the plane of Fig. l(a) were prepared at various positions along the length of the elongated particles. A section taken at position 1 in Fig. l(a) is presented in Fig. l(b). Here, the dark line represents the edge of the sample and the left-hand portion of this photomicrograph is that from the surface perpendicular to the original plane of polish. Since it was necessary to repolish the original surface after each sectioning, the shape of the bainite particles on this surface, right hand side of Fig. l(b), changes with each sectioning. The disappearance of plate A, Fig. l(a), in Fig. l(b) emphasizes the small cross section of these structures. The group of particles in the lower left-hand

Jan 1, 1964

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 William P. Prof. Blake

WHEN we consider the efforts made in Europe to promote the physical and moral well-being of the working classes, the question is suggested whether in this country, where, theoretically, every man is peculiarly the arbiter of his own destiny, we may not be too prone to expect every man to take care of himself, and neglect to make those provisions for the welfare of the employed, demanded alike by enlightened economy and humanity. In the older countries, where the disproportion between capital and labor is greater, and the working classes are more dependent, their welfare largely occupies the attention of employers. The subject is involved in the problem of the just relations of capital and labor, and we are rapidly approaching the time, if we have not already reached it, when a generous paternal interest in the welfare of the employed should be more generally manifested. It is a subject which is of special importance to mine-owners and engineers in this country, especially to those located in the coal regions. My own attention has been particularly directed to it by a visit made to the Hassard collieries, a few miles from Liege, Belgium, under the direction of M. Andrimont. This celebrated engineer has established a comfortable home for the miners near the mouth of the shaft of the mine. It has been highly successful and beneficent in its results, and may to a great degree be regarded as a, model for such undertakings. It is known as "Hotel Louise," this being the name of Madame d'Andrimont, who laid the corner-stone of the building April 4th, 1871. The structure is of brick, upon three sides of a square, and

Jan 1, 1875

By William P. Blake

When we consider the efforts made in Europe to promote the physical and moral well-being of the working classes, the question is suggested whether in this country, where, theoretically, every man is peculiarly the arbiter of his own destiny, we may not be too prone to expect every man to take care of himself, and neglect to make those provisions for the welfare of the employed, demanded alike by enlightened economy and humanity. In the older countries, where the disproportion between capital and labor is greater, and the working classes are more dependent, their welfare largely occupies the attention of employers. The subject is involved in the problem of the just relations of capital and labor, and we are rapidly approaching the time, if we have not already reached it, when a generous paternal interest in the welfare of the employed should be more generally manifested. It is a subject which is of special importance to mine-owners and engineers in this country, especially to those located in the coal regions. My own attention has been particularly directed to it by a visit made to the Hassard collieries, a few miles from Liège, Belgium, under the direction of M. Andrimont. This celebrated engineer has established a comfortable home for the miners near the mouth of the shaft of the mine. It has been highly successful and beneficent in its results, and may to a great degree be regarded as a model for such undertakings. It is known as ((Hotel Louise," this being the name of Madame d' Andrimont, who laid the corner-stone of the building April 4th, 1871. The structure is of brick, upon three sides of a square, and

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 William E. Ford, Edward Salisbury Dana

URANINITE. Cleveite. Broggerite. Nivenite. Pitchblende. Isometric. In octahedrons (o), also with dodecahedra1 faces (d) ; less often in cubes with o and d. Crystals rare. Usually massive and botryoidal; also in grains; structure sometimes columnar, or curved lamellar. Fracture conchoidal to uneven. Brittle. H. = 5'5. G. = 9'0 to 9'7 of crystals; of massive altered forms from 6'4 upwards. Luster submetallic, to greasy or pitch-like, and dull. Color grayish, greenish, brownish, velvet- black. Streak brownish black, grayish, olive-green, a little shining. Opaque. Comp. -A uranate of uranyl, lead, usually thorium (or zirconium), often the metals of the lanthanum and yttrium groups; also containing the gases nitrogen, helium and argon, in varying amounts up to 2'6 p. c. Calcium and water (essential?) are present in small quantities; iron also, but only as an impurity. The relation between the bases varies widely and no definite for- mula can be given. Radium was first discovered in this mineral and it has been shown that it and the helium present are products of the breaking down of the uranium.

Jan 1, 1922

By Franklin Moeller

Discussion of the paper of FRANKLIN MOELLER, presented at the New York meeting, February, 1916, and printed in Bulletin No. 110, February, 1916, pp. 343 to 354. K. A. PAULY, Schenectady, N. Y.-I read with interest Mr. Moeller's paper descriptive of the mechanical parts of the new electric hoist at the Granite Shaft of the North Butte Mining Co. and as the paper treats largely of the mechanical equipment I have little discussion to offer. There is, however, one question which I would like to ask and that is, why the discrepancy in hoisting cycles between the curves given in the paper read by Mr. Sykes for the American Institue of Electrical Engineers at San Francisco and those given in the paper under discussion? In Mr. Sykes' curves the acceleration period is shown to be 16 sec. for all depths from 2,000 to 4,000 ft. inclusive, while Mr. Moeller in Fig. 2 shows 25 sec. throughout the range and in Fig. 4 shows 35 sec. Mr. Moeller's curves also show the following reductions in the peak load during acceleration: Level, Feet Mr. Sykes, Horsepower Mr. Moeller, Horsepower 2,060 3,500 3,130 3,000 3,800 3,480 Fig. 2 4,000 4,100 3,800 2,250 1,595 Fig. 4 As the purchaser's specifications called for 15 or 16 sec. I would like to know whether or not any modifications have been made in the requirements since the equipment has been installed.

Jan 5, 1916

By R. W. Parsons

This discussion concerns fitting an ellipse to angle, where the permeability k is measured for a series of plugs cut from varying angles in the horizontal plane. The conclusions and procedures given by Greenkorn, et al. are in no way affected by these comments, since the degree of anisotropy (ratio of maximum to minimum permeabilities) they found is generally quite close to one (see their Table A-1). However, since large anisotropies may arise, I feel that the comments should be made. Both Marcusl and Scheidegger2 have shown that there are two limiting expressions for the permeability of an unbounded anisotropic media. If the permeability is measured in the direction of the pressure gradient, the result is equivalent to the author's Eq. 11. This is the equation used to find kl1 and k22 from the experimental data. If, however, the permeability is measured in the direction of flow, then the resulting equation for the measured permeability is From these equations it follows that plots on angle will be ellipses. The principal axes will correspond with the major and minor permeability axes. The question arises as to what permeability is actually being measured on an anisotropic sample in the laboratory. An overall pressure gradient and a gross flow rate are determined and a permeability calculated by Darcy's law. The details of the macroscopic flow within the sample will be determined by the boundary conditions of the sample and the orientation and magnitude of the major and minor permeability axes. The situation is shown in Fig. 1 for the two-dimensional case. Using the method of conformal mapping, Marcusl has solved the problem of determining the overall apparent (or measured) permeability for this experiment for any condition of W-L ratios and orientation and magnitude of the principle permeability axes. For W-L ratios approaching zero, the streamlines are all forced by the boundary conditions to be in the direction of the measured permeability which is equal to kg. For W-L ratios approaching infinity, the effects of the no-flow bounds are negligible, and the pressure gradient and measured permeatility direction are parall;l. The streamlines are

Jan 1, 1965

By C. Feng, W. E. Krul

A study was made of the development of texture and the anisotropy in plastic flow of Ti-8Al-1Mo-1V alloy. Based on Pole figure determinations, the shifting of texture induced by rolling at approximately 400°C was found to be due primarily to slip rotation for the major Portion of the material. Grain boundary shear is believed to be an important factor. The anisotropy of the textured alloy was examined in terms of the variations of yield stress under tension and the ratio of bi -axial strain increments µp, in the temperature range 25" to 290°C. The results were related to Hill&apos;s theory on plastic anisotropy. The Schmid factors of (1100)[1120], (1101)[1120/, and (1101)[1120] slip systems were analyzed and found to be compatible with the observed anisotropy. Cross-slip between these planes was proposed as a possible deformation mode. In a number of published articles, considerable interest has been directed to the possible achievement of texture hardening in hcp metals. Following Backofen, Hosford, and Burke,&apos; this phenomenon was related to the yield criteria of the material and was expressed in terms of the biaxial strain ratio, r = d?w/d?l. The higher the value of r, the greater is the expected potential for texture hardening under certain loading conditions. For a given material, r varies with direction. Such variation can be traced to the anisotropy in plastic flow and can be explained within the framework of the various modes of deformation. Hatch2 found that a high r value coincides with a texture whereby the (0001) pole is closely aligned with the surface normal for sheet materials, Based on the analysis of the slip on the {1010}, {1011}, and (0001) planes, Lee and Backofen3 and Avery, Hosford, and Backofen4 concluded that the resistance to thinning is reduced by the operation of the (0001) <1120> slip system; with this reasoning they were able to explain the low r values (i.e., r « 1) observed in magnesium alloy sheets in the rolling direction and in commercially pure titanium in the transverse direction. The general equation, dealing with plastic flow in a polycrystalline aggregate has been used to correlate the plastic anisotropy and texture. In this expression, T and s are shear and normal stresses, and dri and d? are shear and normal strain increments, respectively. Assuming that five slip systems are operative within each grain and applying the principle of maximum work,5,6 one can determine the m value among the available systems. On this basis, Hosford7 and Chin, Nesbitt, and Williams&apos; were able to correlate m with yield stress under plane-strain compression, and Svensson9 was able to predict the variation of yield stress in textured aluminum. These workers made their analyses from materials in which slip operation is known to be associated with plastic flow. Questions remain regarding the derivation of Hill&apos;s theory on plastic anisotropy,10,11 since it was formulated on von Mises&apos; yield criterion.&apos;&apos; Its ability to deal with other forms of deformation has been in doubt.13 Others have discussed the validity of Hill&apos;s quadratic equation relating strain and yield stress.14&apos;15 For hcp titanium, deformation by various modes of slip and twinning operations has been reported.16-20 If all possible modes of deformation operate and contribute substantially to the plastic flow, it is difficult to imagine how the quadratic expression can suitably describe the anisotropic plastic flow of titanium alloys. Backofen and Hosford15 considered that Hill&apos;s is a macroscopic theory and implied that the major mode of deformation by slip mechanism will adequately describe anisotropy of the material. In the present investigation, slip operation will be shown to play the major role in the development of sheet texture induced by rolling of a commercial titanium alloy. Although twinning and other modes of deformation may also operate, their operation is believed to be secondary. The anisotropic properties of the sheet, which can be expressed in terms of directional variation of r, µp = -d?w/d?l and the yield stress will be shown to be governed primarily by slip operation. MATERIALS AND EXPERIMENTAL TECHNIQUES The titanium alloy chosen for the present investigation had a nominal composition of 8 wt pct Al, 1 wt pct Mo, 1 wt pct V, and 0.1 wt pct interstitial impurities. Sheets varying between 0.1 and 0.15 in. thickness were used. The alloy was received in a condition which was prepared by rolling at 900°C and annealing at 700°C. Subsequently, the sheets were subjected to further reduction in thickness by rolling at 400°C. A total reduction in thickness of 65 to 70 pct was obtained by a series of quick passes in a rolling mill with intermediate reheating. Further reduction in thickness was not possible due to cracking developed at the edges of the sheets. X-ray measurements were conducted in a Siemens and a Norelco unit to determine the texture of the sheets. Reflection techniques were used exclusively with CuK, radiation and a nickel filter. The loss of X-ray intensity due to geometric defocusing was calibrated with a technique described previously." The (0001), (1010), and (1071) pole figures were plotted from 0 to 80 deg, and to present the texture elements quantitatively, inverse pole figures were constructed following the technique described by Jetter, McHargue, and Williams.22 Tensile experiments were carried out at 25", 175",

Jan 1, 1970

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 Waldemar Lindgren

Discussion of the paper of WALDEMAR LINDGREN and CLYDE P. Ross, presented at the New York meeting, February, 1916, and printed in Bulletin No. 106, October, 1915, pp. 2171 to 2190. WALDEMAR LINDGREN, Boston, Mass.-I happened to go down to Cuba rather unexpectedly in the winter of 1914, and spent a few very interesting days at Daiquiri and Mayari. To C. F. Rand and his associates I am greatly indebted for permission to visit the mines and for many courtesies received. A few months after that, I met Professor Kemp who informed me that he had just returned from a geological study of Daiquiri. We talked over what to do in a case like that. We both liked to publish our opinions, and so finally agreed to write two papers entirely separately, I not knowing any of Professor Kemp&apos;s conclusions,1 and vice versa. We were rather interested in seeing what would happen. Of course, as might be expected, we disagreed on some points; not, of course, that we ordinarily disagree, but simply because when two men work in the same field and with different ideas, probably they are apt to vary slightly in their conclusions. Some years ago A. C. Spencer went down there for the military interim government and published the results of his study. His view of the origin of the deposit differed from that of Professor Kemp and from mine. So here are three different results obtained by three different geologists. Such differences in opinion on obscure subjects sometimes tend to bring geology into disrepute. It is perhaps not surprising that different opinions have been expressed, for this occurrence of iron ore is one of the most difficult to explain that I have ever seen. MAX ROESLER, Great Neck, L. I.-I had the opportunity this summer of spending about two months down at the Juragua deposits, and studied them with the idea of writing a paper on them, which I hope will come out later. The interpretation of the occurrence at Ocania Mine is the thing which particularly struck me, in the last paper. At the Ocania Mine we may have these large blocks of limestone which have been utterly and entirely altered, to a remarkable extent.

Jan 5, 1916

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

Discussion of the paper of Edward Keller, presented at the Butte meeting, August, 1913, and printed in Bulletin No. 80, August, 1913, pp. 2093 to 2115. GEORGE L. HEATH, Hubbell, Mich.:-In the admirable paper quoted, is mentioned the date when the 5-g. assay was first proposed is a standard for refined metal. The author omitted, however, to mention a later paper,1 which contains a proposal for the use of a single " stock solution " of mixed acids, which has been adopted by the American Brass Co. and others. The suggestion is made that such a scheme would save time and manipulation with converter metal. Unless the low current of 0.5 ampere and the large excess of nitric acid, recommended by Mr. Keller, have been proved necessary to hold up antimony-and selenium, the use of the mixed solution which we have adopted will permit the use of 1 ampere of current per square decimeter of cathode surface, until the solutions have become colorless. At this point, we wash the covers and reduce to 0.5 ampere to prevent oxidation or contamination. The ordinary split electrodes have been used. With strong current, at least, the use of an excess of nitric acid tends to the neutralization of the solution before the end of the period, from the formation of too much ammonia., and this is detrimental. Antimony deposits more easily than arsenic, and tends to drag the latter dorm with it. There must, be some such explanation for the fact. that we have made hundreds of deposits of pure cathodes from Lake material containing no antimony, but as. high as 0.5 per cent. of arsenic. By placing an assay beaker in the Frary solenoid, or rotary device, a cathode deposit with less than 0.01 per cent. of impurity is easily obtained in one operation from 3 g. of whitneyite, carrying from 7 to 10 per cent. of arsenic. In such a case, it is necessary to test several times for end point and remove the plate as soon as no brown tint appears (at once) when hydrogen sulphide water is added to the test portion on the spot plate. Edward Keller&apos;s proportion,, of solvent figure out as 14 cc. of strong nitric to 11.4 cc. of sulphuric acid (1.84).

Jan 11, 1913

By C. L. Dake

Discussion of the paper of. C. L. DAKE, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 103, July, 1915, pp. 1429 to 1436. A. C. LAWSON, Berkeley, Cal.-It appears that our bog-iron ores are due in a large measure to the activity of certain iron bacteria, and a paper dealing with this subject that makes no reference to that particular agency strikes me as rather curious. C. L. DANE, Rolla, Mo.-Mr. Lawson&apos;s criticism that this paper makes no reference to the activity, of iron bacteria is scarcely true. On p. 1430 I stated: "Certain bacteria precipitate iron by building the hydrated oxide into their body cells," and again, "There are many other means by which, under special conditions, iron may be precipitated in nature. Oxidation, evaporation of CO2, and iron bacteria have been held to be the most important." Thus the activity of bacteria receives as extended mention as the action of any other agency in precipitation of iron. The paper makes no pretense of covering exhaustively the origin of bog ores, but, as its original title suggested, refers to Some Principles Controlling the Formation and Distribution of Bog Iron Ores. Mr. Lawson seems to have entirely missed the main thesis of the paper, which attempts to establish some relation between glaciation and abundance of bog ores now forming. Unfortunately, I have no immediate access to the literature of the subject, but my best recollection is that the data regarding iron bacteria throw no light whatever on the cause of bog ores being so much in ore abundant within the limits of the glaciated regions, and being reported much less frequently from the tropics. This lack of data is suggested in the following (p. 1434): "It has already been shown that bacteria aid in the precipitation of iron. Whether tropical conditions increase or decrease the activity of such bacteria is unknown."

Jan 12, 1915

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 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 D. Weinstein, F. C. Holtz

AS a possible method of improving the elevated temperature strength properties of zirconium, an investigation was initiated on the feasibility of producing a dispersion-strengthened material. Because of the high reactivity of zirconium, its high solubility for oxygen, and the stability of the Zr-0 solid solution, the major problem in such a development is choice of a suitable dispersant. Thus, in the present investigation we were concerned primarily with the stability of various dispersants in the zirconium matrix. The experimental procedure consisted of blending powders of zirconium and a dispersant, followed by cold compaction and extrusion. The best available source of -325 mesh zirconium powder contained between 1500 and 3500 ppm Oz; to this material, powders of zirconium carbide (5 p max), vanadium carbide (5 p max), alumina (0.03 p average), lan-thana (0.8 to 2 p), ceria (0.8 to 2 p), yttria (0.8 to 2 p), calcia (44 p rnax), or thoria (0.6 to 0.8 p) were added in amounts of 7 vol pct and compacted at 65 tsi. A cylindrical compact having a density between 70 and 80 pct of theoretical and dimensions of 1 in. diam by 1-114 in. high was thus produced. After canning in copper, these billets could be extruded (5: 1) on a 54-ton capacity, slow-traverse hydraulic press with the billet temperature at 1550°F and the extrusion die at 900°F. However, lack of densifica-tion of some of the extruded billets necessitated ratios of at least 23 :1. Ultimately, all billets were successfully extruded at 1500°F to 0.190 in. diam (32 :I), fully dense rods using a 200-ton capacity press and a ram speed of 90 ipm. The microstructures of as-extruded Zr-7 vol pct LazOS and Zr-7 vol pct Y2Os are shown in Fig. l(a) and (c), respectively. These structures are similar to all the as-extruded materials and consist of an elongated, single-phase zirconium matrix dispersed with oxide or carbide particles. Very little porosity is observed, and the interface between matrix and particles appears satisfactory. The size and distribution of particles, however, are not ideally of the type desired for dispersion strengthening. Since the primary study was of particle stability with respect to zirconium, no attempt was made to overcome agglomeration during powder blending and fabrication. Some areas exhibit fine, well-distributed particles; undoubtedly, a small proportion is submicroscopic and has the

Jan 1, 1963

By AIME AIME

T HE Board of Directors of the A. I. M. E. held a meeting at Institute headquarters on Jan. 28, 1921. There were present 10 directors and 14 guests, the secretary and the assistant secretary. The following actions of the Executive and Finance Committees were approved: Wilkes-Barre Meeting, Sept. 12 to 17, 1921; authorization of Oregon Section; authorization of Upper Peninsula Section; appointment of Philip W. Henry and Thomas H. Leggett on special committee on Code of Ethics; and presentation of five copies of Raymond Memorial Volume to T. A. Rickard, who edited it. The By-Laws of the Ohio Section were approved. The resolutions in reference to the payment of certain contributions and assessments to the Library Board of the United Engineering Societies, adopted by the Board of Directors on June 27, 1919, were rescinded, and the resolution adopted that the income of the James Douglas Trust of $100,000 be paid over to the Library or otherwise applied by it for the purpose of maintaining the Scientific Library of this Institute in such manner as may be deemed advisable in furtherance of the purposes of such trust, and that said income shall be paid on account of and included in. the assessment levied by the United Engineering Societies on the Institute for the maintenance of the joint libraries of the Founder Societies.

Jan 1, 1921

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.&apos; Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-&apos; and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964

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