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By M. C. Smith, W. V. Green, D. M. Olsen

The creep-rupture behavior of commercial powder-metallurgy molybdenum rod is reported in the temperature range 1600" to 250O°C, at stresses up to 9000 psi and times up to 1 month. The effects of temperature, stress, and grain growth are discussed. Rupture time is fitted to the Larson-Miller parameter and compared to lower-temperature and higher-stress results reported by pugh.1 BECAUSE of its high melting point, molybdenum should retain useful strength to relatively high temperatures. Combined with its ready availability in the United States, this makes it attractive for many applications in missiles, rockets, and so forth—wherever its susceptibility to oxidation can be tolerated or overcome. The mechanical properties of molybdenum rod in the temperature range —200" to 1540°C have been reported by pugh,' Bechtold,' Parke,3 and Carriker and Guard.4 Madden and chen5 have measured the tensile properties of molybdenum single crystals in vacuum up to about 2500°C. As one further step in evaluating its mechanical usefulness, the constant-load creep-rupture properties of commercial powder-metallurgy molybdenum rod have been investigated in the range 1600" to 2500°C. MATERIAL TESTED Creep specimens were machined from 1/2-in. round commercial molybdenum rod, manufactured from powder by pressing, sintering, and swaging. Spectrochemical analysis of the rod showed "traces" (less than 0.01 pct) of silicon, aluminum, chromium, iron, and zirconium, and "faint traces" (less than 0.001 pct) of manganese, magnesium, cobalt, and nickel. Carbon content was 130 to 200 ppm, nitrogen was 110 to 180 ppm, and oxygen 30 to 35 ppm. A typical microstructure of the as-received rod is shown in Fig. 1. Room temperature tensile properties for five specimens strained at about 0.015 in. per in. per min are shown in Table I. CREEP SPECIMENS USED The specimens used for creep-rupture testing are illustrated in Fig. 2. The 1/4-in.-diam gage section was 3/4 in. long, and terminated at shoulders 5 mils high. These shoulders served as fiducial marks for optical strain measurements. Surface finish on the gage section was 16pin. r.m.s. One specimen, for a "long-time" test described below, was modified by dividing the 3/4-in. gage length into three 1/4-in. long sections with individual diameters of 0.250, 0.230, and 0.210 in., each terminating in a pair of fiducial shoulders. TESTING PROCEDURE The constant-load creep-testing machine used has been described by Smith, Olson, and Brown.6 In it the specimen is held vertically on the axis of a cylindrical tantalum or tungsten heater tube by threaded molybdenum or tungsten grips. Both specimen and grips are heated by radiation from the heater-tube, which is heated by its own electrical resistance. The bottom specimen grip is held at its lower end by a clevis pin. The testing load is applied to the specimen through the upper grip by means of hanging weights, a constant force-multiplication lever system, and a pull rod sealed to the chamber lid by a bellows. The incandescent specimen is viewed by an external optical system through slots in the heater-tube and radiation shielding, and an enlarged image of it is projected on a ground-glass screen. Gage-length measurements are made on this image with a pair of cathetometers. Thorium oxide coatings were applied to the threaded ends of most specimens, to prevent diffusion-welding of specimens to grips during testing. Without such a coating welding usually occurred, and grips were often broken by subsequent efforts to remove the tested specimens.

Jan 1, 1960

By R. S. Wagner, R. G. Treuting, W. C. Ellis

Use of the Weisseizbevg goniometer for the study of the morphology of whisker crystals and transfer of the results to a stereograplzic projection are described. While in almost all instances a complete and rapid solution is obtained with a purely gaphical treatment, an absolute analytical treatment applicable to difficult cases is given. Examples are given for determination of growth direction and external features of a crystal, for detection of 'twintzittg, and for establislting the orientation relntionships in a kinked whisker crystal. We give here a method for the use of the Weissen-berg goniometerl" in the study of orientation relationships in "whisker" (micro) crystals3-8 and direct transference of the data to the stereographic projection. The operations are straightforward and require no involved calculations: in almost all cases solely graphical treatment is adequate. In a few complex instances, a more exact analytic method may be required. In the method, not only are equatorial reflections of an oscillation photograph used, but also those on higher layer lines, or those not occurring on a recognized layer line. Such reflections off the zero level are often essentialy to detect the presence of twinning. The method is particularly suitable for examination of whisker crystals since the axial or growth direction is almost always one of high symmetry, permitting a more restricted oscillation range to obtain the necessary reflections and an accordingly shorter exposure time. The method is also applicable when there is no lattice-related external symmetry, and is as well able to identify external crystal surfaces, when such exist, with the aid of an optical beam. Thus growth direction, identification of lateral faces, twinning, and orientation relationships in a kinked crystal can be established. A test for the Eshelby twist6-8 can readily be made. The method can be used for orientation, for structure analysis, and as an aid in the identification of an unknown crystal. Moving-film techniques have previously been employed variously for crystal-orientation studies.1,2,9-13 In particular, use of the Weissenberg method for orientation determination has been reported by Wooster and wooster.14 While their method derives the same data as here described, it differs in depending on the tracing of constant p streaks, a less than dependable phenomenon with small specimens, a few microns or less in cross section. The Laue method can and has been used for orientation studies of microcrystals,15 e.g., 2 p in cross section, but requires the extreme intensity and concentration from a microfocus tube to obtain reasonable exposure time. PRINCIPLES OF THE PRESENT METHOD Consider a crystal of random orientation with respect to the oscillation axis in a Weissenberg goniometer. Its diffraction pattern need not necessarily result in recognizable layer lines. In Fig. 1, a stereo-graphic projection of the reference sphere is given with the equatorial plane XZ normal to the oscillation axis Y, and the X-ray beam directed from X towards 2. The great circle ZZ is then normal to the beam, and the axes are right-handed. Thus the reflected X-ray beam lies at the intersection R of small circle ARB of radius 28 from 2, and of small circle RE of radius a from the rotation axis Y. a is the conventional semiapex angle of a cone of diffracted rays from the atoms aligned in the direction

Jan 1, 1967

By W. A. Rachinger, C. Graeme-Barber, R. L. Bell, R. C. Gifkins, T. G. Langdon

R. L. Bell. C. Graeme-Barber, and T. G. Langdon (Imperial College. London)— The internal-marker technique developed by Ishida, Mullendore, and Grant has enabled them to make some interesting observations on the role of grain boundary sliding in creep. Certain of their conclusions are supported by our own similar experiments on Magnox AL80 (Mg-0.8 pct Al) specimens containing several markers, full details of which will be published shortly. In particular, we would agree that: 1) Using the internal-marker method, there is little difference between Egb, the contribution made by grain boundary sliding to the total strain, measured at the surface and in the interior of a specimen. 2) The measurement of the change in grain shape during creep leads to an underestimation of the grain strain, and hence an overestimate of Egb.. However, the discrepancies between the values obtained by this method and those obtained using markers are not as great as Tables IV and V of Ishida, Mullendore, and Grant would suggest; see below. The authors' Eq. [I] which is used to compute Egb from the transverse displacement ITt of longitudinal marker lines is not given in the reference quoted,'' where in fact only relations for Egb in terms of the longitudinal displacements of markers were developed. As first pointed out by Gifkins and Gittins,12 a problem arises in the use of longitudinal markers. and we will show that Eq. [1] underestimates Egb in the interior by a factor of 2. In Fig. 12, two grains X and Y have become displaced by the vector AC which lies in the plane of the grain boundary ABCD separating them. A longitudinal marker has been split by this displacement into the two parts LA and CAW. If these were surface grains the transverse displacement, Ut. could be obtained by viewing normal to the "top" surface. If interior, a section through CD parallel to the top surface would show the same result, provided the longitudinal internal markers delineated planes normal to the top surface. (This is an essential feature of the markers not pointed out in the paper.) The important point is that the quantity Ut tan B (=BE=DF) only gives the elongation due to the one component AB of the sliding. The elongation V/tan 8 (=GD) due to the component AD must be added to produce the total elongation resulting from the boundary displacement AC. If the grain boundaries in a poly crystalline specimen are randomly oriented with respect to the stress axis it follows that In the interior of a specimen the two sums depend for any difference simply on the definitions "top'' and "side". On the surface it is possible that the two sums could differ somewhat. In either event it is clear that the authors' Eq. [I] underestimates Egb, and in the interior, and perhaps at the surface also, the appropriate formula is given by The suggested modification probably makes little difference to the comparison between surface and interior values of Egb where both were obtained from marker measurements. For the estimation of the correction becomes extremely important where the boundary contribution is large. In our own work on magnox, for example, we have obtained values of as large as 70 to 80 pct, under conditions of high temperature and low strain rate. The use of planar markers transverse to the stress axis would simplify the comparison between surface and interior behavior, because measurement of the longitudinal offsets Us of these markers could be summed to give the total elongation di-

Jan 1, 1965

By J. Leslie Goodier

The International Law of the Continental Shelf, so far ratified by 35 nations, extends the national boundary of any coastal nation to the edge of the continental shelf, this normally being at a continuous water depth of 200 m. The Law further extends this boundary to include the floor of the deep ocean to any depth that can be mined by advanced mining technology. In effect, proof of mining can constitute proof of ownership of the subaqueous land and the minerals on or below the sea floor. Irrespective of the fact that present technology is too limited to permit mineral exploitation in the high seas-and the law regarding the right to mine appears hazy-the U. S. Treasury Department's Bureau of Customs, has a ruling that would further deter mining operations on the high seas. This law contends that minerals mined on the continental shelf of the United States are actually mined within the continental United States and are free of tariff, but mined products or other articles obtained from the ocean or the sea floor beyond the continental shelf, if brought into this nation, must be considered as imported and are subject to such customs duties as are applicable under the tariff schedules of the United States.

Jan 7, 1968

By A. M. Rowe, I. H. Silberberg

A computer program was written to predict the phase behavior generated by the enriched-gas-drive process. This program is based, in part, on a new concept of convergence pressme, which is then used to select vapor - liquid equilibrium ratios (K-factors) for performing a series of flash calculations. The results of these calculations are the equilibrium vapor and liquid phase compositions which define the phase envelopes. The program was used to predict phase envelopes for 11 different hydrocarbon systems on which published experimental data were available. The predicted and experimental results compare favorably. INTRODUCTION The reservoir engineer is frequently faced with the problem of predicting what will happen if gas is injected into a reservoir. One aspect of this, general problem is predicting the phase changes that will occur when a non-equilibrium gas displaces a reservoir fluid. In particular, a "dry" gas, upon displacing a volatile oil, will pick up intermediate components from the oil. On the other hand, a "wet" gas, containing a high concentration of intermediates, will lose some of these components to a relatively low-gravity, non-eouilibrium1- crude. It is this latter Drocess. occurring in the enriched-gas displacement, which is treated in this paper. In the past, these phase changes have been determined experimentally and the results incorporated into various modifications of the Buckley-Leverett analysis.112 Such experimental work is time consuming, and the results are sensitive to numerous experimental errors. With the wide availability of high-speed digital computing equipment and numerous correlations pertaining to the vapor-liquid equilibria of hydrocarbon systems, it is now practical to calculate such phase behavior. This paper describes a computer program for performing these calculations. THE ENRICHED GAS DISPLACEMENT PROCESS Experimental results have shown that oil recovery can be significantly increased by enriching the displacing gas with intermediate hydrocarbon c0m~onents.3 The essential features of the phase behavior generated by this enriched-gas-drive process are commonly illustrated with ternary diagrams such as Fig. 1.4 In this figure, Gas D, which contains a high concentration of intermediate hydrocarbons with respect to the undersaturated Crude A, is injected into the reservoir. When D contacts A, gas goes into solution until the oil becomes saturated (Point. B). Further contacting of Gas D and saturated Oil B results in a Mixture C which separates into Vapor Y(c) and Liquid X(c). Liquid X(c) is contacted by additional Gas O, resulting in Mixture E which separates into Vapor Y(e) and Liquid X(e). Repeated contacts of the liquid by the injected gas will eventually result in Liquid X(4 of maximum enrichment existing in equilibrium with Gas Y(d). The equilibrium tie-line X(4 Y(4, when extended, passes through the Point D representing the enriched injection gas. For systems of more than three components, the predicted equilibrium states are dependent upon not only reservoir temperature and pressure, but also the compositions of the crude oil and injected gas. If the gas is sufficiently enriched, a miscible displacement is generated. Line If is tangent to the phas,e envelope at the critical point (Point Z) and represents the limiting slope of the tie-lines as the critical state is approached. Point 1 therefore represents the minimum enrichment of injection gas required to generate a miscible displacement. Point G represents the minimum enrichment required for initial miscibility of the injection gas with Crude A. Accra has presented a method to be used for prediction of oil recovery by the enriched gas displacement process.l To develop the phase behavior data needed, he designed the experimental procedure described in the following quotation from his paper: The original liquid was contacted by a volume of displacing gas and allowed to come to equi-

Jan 1, 1966

Albert Arents, Alameda, Cal.: From Mr. Furman's description of his crucible-assays I infer that he regards iron nails as a necessary or advisable adjunct. Against such a notion I must beg leave to protest. Nails should not be used in

Jan 1, 1896

Extremes in temperature and weather, along with the highly corrosive nature of acid leach solutions used at open-pit copper mines, necessitates the use of pipeline systems that are both corrosion resistant and impervious to the environment.

Jan 6, 1976

R. E. Powers (Mellon Institute of lndustrial Research, University of Pittsburgh, Pittsburgh)—Several of the processing methods at the Josephtown smelter might well be considered by plants producing iron blast furnace sinter. In making blast furnace sinter the objectives are much the same as at Josephtown: To produce a strong yet porous agglomerate which has a size consist in a preferred range. The emphasis however is on production rate rather than on the size or other quality characteristics of the sinter. Therefore the technique is entirely different. Blast furnace sinter plants attempt to make their product in one pass with a minimum recirculating load and without sizing treatment after the sinter leaves the machines. Many plants are beginning to feel that more attention paid to quality characteristics would make the product a more desirable blast furnace material. The pelletizing of very fine material before placing it on the bed is not deliberately done at iron sinter plants, although the installed equipment sometimes gives a simila; action. Such pelletizing seems to be a promising way of accommodating the down-draft sintering Drocess to very fine materials. he recirculating load at Josephtown is extremely high. Two plants' producing blast furnace sinter from raw material of comparable size have a recirculating load of about 100 pct of production. At Josephtown it is notable that the size and the rate of feeding of return fines are under control. This is not the case in most blast furnace sinter plants. The sinter slicer appears to be a worthwhile aid in effecting such control. It is similar in action to rakes and plows used at a number of plants, but it has the advantage that the sinter dislodged is positively removed and not left to the inefficient action of a stationary grizzly screen. Blast furnace size specifications for sinter are not at present so rigid as the Josephtown specifications. If the sizing of blast furnace sinter does become important, then the Josephtown crushing practice, in which a large recirculating load is maintained on the crusher in order that minimum fines be produced, may be of interest. H. K. Najarian (authors' reply)—We note that Mr. Powers appreciates some points that we tried to emphasize in our paper as being of importance in making zinc sinter of good quality and which may well be applied to iron blast furnace sinter. Fig. 2 shows the pelletized nature of the feed going on to a Dwight-Lloyd type sintering machine in our plant. Practically, the entire feed consists of more ,or less rounded particles which permit more uniform air passage through the charge, while the larger particles in the charge roll on to the surface of the grate, which helps to keep the grate openings from being clogged by excessive fines. An agglomerated charge of this character may preferably be made by rolling action while being mixed in a rotating drum and wetted by water sprays to bind the fine particles together and give the charge the desired moisture content. From our observations of several iron ore and blast furnace flue dust sintering operations, we believe that if the fines from the sinter discharged from the machines were to be recirculated and agqlomerated with the new feed, not only sinter of better quality but larger capacity from the machines may be realized.

Jan 1, 1952

* Kennecott Copper Corp. gets Charles R. Cox as president on Jan. 1. Mr. Cox is resigning his position as president of Carnegie-Illinois to take the new post with Kennecott, left vacant by the death of Mr. Stannard in September. •The ECA signed a contract in December to advance X3,600,000 to Newmont Mining Corp. to aid development of lead and zinc mines in French Morocco. The funds are to be repaid in lead and zinc for the United States' stockpile over a period of seven years. The mines are owned by the Societe des Mines de Zellidja, with which organization Newmont is associated. • Under the direction of John M. Brooks, Jr., general manager, the Matahambra mine in Cuba, will probably produce sufficient tonnage to make 4 million lb of copper per month during 1950. The grade is presently running between 7 and 10 pet. •S. H. Ash reports that the fatality rate per million-man-hr for the anthracite industry for 1949, through November, is 0.78. This is 15 pct better than that achieved during 1948, which was the lowest fatal injury rate in coal mining history. The first full year on record without a major disaster was recorded in 1949 (p. 34). •The Atomic Energy Commission has authorized the production of 200 lb of uranium metal for use under AEC license in non-Commission research projects. •A national survey of projected 1950 purchases of new machine tools, machine tool accessories, materials handling equipment, etc., just completed by the American Society of Tool Engineers reveals that, of the companies reporting, 80 pct state that they plan to buy either more equipment or the same amount as in 1948. • Armour Research Foundation is conducting investigations for the use of clay and shale deposits to make lightweight aggregates. The material is heated until it expands and forms material suitable for mixing with cement which it is hoped will be lighter, stronger, have better insulating qualities and will lower the cost of concrete. •In the first six months of 1949 the bituminous coal miners' average hourly earnings were $1.94 -as compared with X1.392_ national average for all manufacturing. Average annual earnings of full-time employees in the bituminous coal mines in 1948 were $3387 as compared with $2809 for all industry. •LaSalle Business Bulletin reports: "year ends on a rising trend in industry and trade ... nearly record-breaking demand from almost all sources keeps business high... most indicators but little below postwar peak... forces keeping activity high arestill powerful--changes in general business conditions likely to be slow and moderate." •Office of Internal Trade of the Commerce Department requests that technical data significant to the national security which is to be sent outside of the United States be submitted to it for an official opinion on the desirability of transmitting such information. This voluntary compliance program is part of our national security control. • Blast furnace slag reduced to 12 to 16 mesh is being used for sanding track at the Mont Coal mines of Armco. The slag replaces silica sand which caused silicosis. It has proved so effective and cheap that tests are being made to use the slag for rock dusting.

Jan 1, 1950

By R. E. Cole, A. M. Gaudin

OLEIC acid, a standard flotation reagent, has generally been preferred to other fatty acids. Because oleic acid differs from saturated fatty acids by the presence of one carbon-to-carbon double bond and because the flotation operation is one in which extremely intimate exposure of the reagent to oxygen is obtained, it appeared possible that the value of oleic acid as a flotation collector was related to the oxidizability of its double bond. To test this hypothesis, the floated mineral, fluor-ite, was leached with a solvent capable of extracting the adsorbed reagent and the extract was analyzed.' Results show that oleic acid is not oxidized during flotation, although some oxidation can be obtained if the flotation operation is repeated many times and if oxygen in place of air is employed as the gas during flotation. Incidentally, it was found that lino-leic acid which has two nonconjugated double bonds is not affected appreciably more than oleic acid. Linolenic acid which has three nonconjugated double bonds is measurably altered even during one flotation step, using air. The fatty acids used, from the Hormel Foundation, were of the highest purity. The quantity of fatty acids employed in each test was sufficient to float the mineral, but less than the theoretical amount required to form a monolayer at the mineral surface. The purpose of this limitation was to eliminate droplets of oil smeared on the adsorbate-covered mineral surface. The mineral was dried in vacuum at about 60 °C. Effective leaching was obtained by use of a solution of 1 pct hydrochloric acid in absolute alcohol. The extract was separated from the solvent by distillation, with final recovery of the extract in carbon tetrachloride. The identity of the extract was tested by a combination of analytical procedures including infrared spectroscopy, saponification number, iodine number, and index of refraction. At the outset, great hopes for accurate quantification of oleic acid oxidation had been entertained in regard to the method of infra-red spectroscopy. Unfortunately, because the double bond in the oleic acid is so sym- metrically located at the center of the molecule that it provides very weak absorption bands, accurate quantitative analyses were not obtained. Nevertheless, infra-red spectrograms suggested the absence of double-bond oxidation during flotation. Iodine number, semi-micro method, provided a critical test of the extent to which fatty acids oxidized during flotation, see Table I. The index of refraction was used in a qualitative rather than quantitative fashion, and its findings corroborated those obtained by the iodine-number method. It is concluded, in the case of fluorite and C-18 fatty acids having one or two nonconjugated double bonds, that there is practically no change of the fatty acid molecule or ion during the flotation operation. It would appear, therefore, that the extraordinary utility of these reagents is related to some property of the compounds other than the oxidizability of their double bonds. Acknowledgment The research reported herewith was sponsored by the Research Division, U. S. Atomic Energy Commission, and for this help the authors express their appreciation. Reference 'R. E. Cole: "Double-Bond Reactivity of Oleic Acid During Flotation." Thesis submitted in partial fulfillment of the requirements for the degree of M.S. at the Massachusetts Institute of Technology.

Jan 1, 1954

In the death of Major A. B. desaulles at South Bethlehem, Pa., on Dec. 24, 1917, the Institute lost a valued and esteemed member, one of the last few of those who, in May, 1871, at Wilkes-Barre, attended the first meeting of the Institute, in response to a call that had been issued by R. P. Rothwell, Eckley B. Coxe, and Martin Coryell. Major desaulles was born Jan. 8, 1840, at New Orleans, and was the son of Louis and Armidc Longer desaulles, each of French descent. As a boy he was privately tutored in the South, and then schooled in New England to enter the Rensselaer Polytechnic Institute, where he was graduated with honors in the class of '59. Following his graduation he studied in France and Germany for two years, returning to New Orleans in 1861 to enter the Confederate Army, in which he served with distinction as an engineer throughout the Civil War, rising to the rank of Major and the command of his Corps. After the close of the war he pursued his studies abroad for another year, returning to New York in April, 1866, when he became engineer for the New York & Schuylkill Coal Company, and remained at its plant near Wilkes-Barre until October, 1871, when it was sold to the Philadelphia & Reading Coal and Iron Company. He then returned to New York where for several years he was engaged in the practice of his profession. In 1869, he married Catharine M. Heckscher, daughter of Charles Heckscher of New York City. Mrs. desaulles survives him. In 1876, Major desaulles became superintendent of the Dunbar Furnace Company in Fayette County, Pa., with which company he remained until 1883. As a feature of the Pittsburgh meeting in May, 1879, Major and Mrs. desaulles entertained the members of the Institute at dinner at Dunbar on the occasion of the Institute's visit to Dun-bar furnace. In 1883, he took up the formation of the Oliphant Furnace Company in that county, of which he became and remained the head for five years. He was then called to the superintendency of the New Jersey Zinc Company at South Bethlehem, Pa., in which position he remained until his retirement,from active service in 1911, maintaining, however, hi.; keen interest in the metallurgy and smelting of zinc, in collaboration with his son Charles, a member of the Institute and a Director of the American Smelting and Refining Company. From 1888, until his death, he resided in South Bethlehem, a prominent and highly respected citizen of that progressive and stirring community. Major desaulles was a member of the Protestant Espicopal Church, and at the time of his death was a vestryman of the Church of the Nativity at South Bethlehem. He was president of the Men's Club of the Church of the Nativity. His kindly nature led him to take an active interest in the promotion of healthful sports among young men. He was ever active in all things pertaining to the general welfare and uplift of his fellowmen. In his death the profession has lost a distinguished engineer and mctallurgist and our country a patriotic able citi-zen and man of affairs—one greatly beloved by those whom he honored with his friendship, and respected and looked up to by all who were privileged to know him.

Jan 1, 1920

By H. E. Stauss, E. I. Salkovitz, F. W. von Batchelder

EXISTING information regarding the structure of a spherulite in nodular cast iron is based on optical studies. According to these data, a nodule consists of an aggregate of graphite crystallites radiating from the center, with the closely packed basal planes at right angles to the radii. The c axes lie along the radii. This view faces some uncertainty in the fact that the c axis does not represent the accepted direction of fastest growth in graphite. To supplement the optical information, X-ray studies have now been made. The principle used was to screen the nodule in greater part from the X-ray beam and expose only a minor cap. As successively larger portions of the nodule were introduced into the X-ray beam, any differences in the X-ray patterns could be observed. Such photographs have been taken with chromium radiation and a Laue camera. The graphite nodule itself, about 0.010 to 0.025 in. in diam, was mounted with vaseline on a micrometer screw for control of the linear motion. The nodule rotated about 45" each time that it was translated linearly. The nodules were obtained from magnesium-treated hypereutectic iron by electrolytic solution of the iron in hydrochloric acid. In Fig. la is shown the pattern of the thinnest cap examined. In Fig. lb is shown the pattern of the same nodule moved 0.003 in. farther into the X-ray beam, and rotated 45" at the same time. Figs, la and lb indicate incomplete circles for graphite (the two outer circles arise from graphite) with the side arcs much weaker than the top and bottom ones. The arcs obtained are themselves not continuous in intensity but vary with maxima of intensity some 15" and 30" apart. The structure of the nodule that would give rise to such a pattern can be explained as follows. Basically the nodule consisted of small crystallites. The discontinuous character of the diffraction rings demonstrates that the nodule was not composed of randomly oriented crystallites. The strong vertical reflections and the weak lateral reflections show that the reflecting planes were roughly normal to the radii. The absence of sharp reflection spots suggests that the nodule did not contain large crystals. The sharpness of the diffraction rings in their radial direction shows that the variations in intensity along the arcs were not the result of line broadening resulting from extremely small crystals. In the diffraction patterns two rings corresponding to graphite were found. The third and inner ring in the figures originated in the vaseline. The graphite rings correspond to the a and ß lines reflected from the basal planes, showing that the radii of the nodules are the [0001] direction normal to the basal planes of graphite. The picture of the structure that is formed is, therefore, one of aggregates of crystallites. Within each aggregate the c axes of the crystallites tend to align themselves in the radial direction of the nodule, although these axes deviate somewhat in direction by a continuous variation of angle. Correspondingly the basal planes of the graphite crystallites are generally normal to the radii. It is a pleasure to acknowledge the assistance of M. C. Bloom and R. P. Dunphy of this laboratory.

Jan 1, 1952

By H. H. Rachford, W. P. Schultz

The use of computing machines to solve physical problems has made it imperative to represent physical data in a form computing machines can use. Although curve-fitting is an old and well-practiced art, there still seems to be some interest in questions regarding what methods can be used and why. Even though there are many good references on this subject, it may be of some value to discuss a particular method which has been found to be useful, and to make available the associated tables for its use in the hope that there can be saved a few of the tedious hours necessary to reduce many of the suggested methods to practice. Although a very brief discussion of the mathematical background of the tables is included immediately below, those interested only in their use can skip directly to the section on Use of the Tables. Direct Fit of a Set of Points A frequently encountered problem is: Given data which can be represented by a smooth curve +(x), to find an easy-to-evaluate function F(x), with only a few coefficients, which is a good approximation of +(x) on the interval 0 5 x 5 x,,. Consider F(x) as a linear combination of m + 1 arbitrary, single-valued, continuous, linearly independent functions, f,(x), Ff.r) = a,f,,(x) + a,f,(x) + . . . -+ aifi(x) + If the value of Q(x) is known or can be read from the curve at the points xj: +(x,), +(x,), . . . +(xj) . . . +(x.), and if n = m, then all the coefficients of F(x) can be determined, and F(x,) — +(x,) = 0 for j =. 0, 1, . . . n. This follows from the solution of the set of linear simultaneous equations. +(x<.) = aofu(x,) + aJI(x0) + . . . + a,,f,,(x,) =a, = f,,(x,) + a,f,(x,) + . . . + a,f,,(x,) +(x,,) = a,,f,(x,,) + a,f,(x,) + ... + a,,f.,(x,,) ...........(2) for the coefficients ai. Although the set a, from the solutions of the set of Equations 2 yields an fix) which gives an exact value of $(x,) for the n + 1 points, there is no restraint on ~(xj in the interval xi < x < xj+,. Indeed, if the points +(x,) are not sufficiently smooth, very serious differences may arise between F(x) in the interval and the smooth curve +(x). Least-Squares Fit It has been suggested&apos; that if n is made to exceed m, and the set a, is found to minimize the function the function F(x) is much less sensitive to small errors in +(xi), and usually provides a much better fit to the smooth function +(x). This is known as the best fit in the sense of the least-squares error. To minimize $, set £ = 0,i = 0,1,... iTi,.....(3) The m + 1 equations from Equation 3 are k—n k=n a.^p /,,(a) f,(xt) + a, X A: = 0 k=O k = n k = n k=0 k=0 +(x.) f,(x,),............(4) one equation being obtained for each i = 0, 1, . . . m. Inasmuch as the arbitrary functions f(x) may be evaluated for x,, k = 0, 1, . . . n, and the +(x,) are known values of the curve to be fitted, the simultaneous Equations 4 may be solved for the set a,. Particular Functions Given the functions fi(x) and the set +(xj), the solutions for require evaluating a number of sums of products as well as the solution of an m + 1 order set

Jan 1, 1956

By D. H. Thompson, A. W. Tracy

E. A. ANDERSON*—At the outset, I note that you are using a humid atmosphere containing ammonia but that you make no reference to the variable of carbon dioxide content. Edmunds in his work in this laboratory found very marked effects on the rate of failure due to variations in carbon dioxide in the environment. This point is, of course, strongly related to the overall corrosion rate problem since the role of the carbon dioxide seems to be to permit the formation of hygrogroscopic salts which give a controlled moisture film on the specimen surface, which in turn seems to support the intergranular penetration more consistently than would otherwise occur. (2) Your results with various copper binary systems are very striking. It is curious, however, that the time-to-failure minima all occur at percentages of the alloying element which are considerably below the solubility limits as given in the conventional equilibrium diagrams. If your theory regarding the presence of these impurities in some concentration in the grain boundaries is correct, then either the existing diagrams are not accurate in the room temperature region, or there is a difference in solubility in the grain boundaries as compared -with the grains. A study along these lines might be very revealing. (3) The undesirable effect of silicon in copper calls to mind our own observations on the influence of silicon on the stress corrosion cracking resistance of alpha brass. In this case, silicon was found to have a very marked beneficial effect, particularly when a heat treatment capable of producing a grain boundary constituent was used. I should appreciate it if in the discussion of your paper this point should arise, you would attempt to clarify the difference between the copper-silicon binaries and the copper-zinc-sili-con ternary alloys. D. H. THOMPSON and A. W. TRACY (authors&apos; reply)—(1) We have no data on the constancy of the carbon dioxide content of the air used for the test atmosphere but have believed that the normal carbon dioxide content of the air was as constant as could be obtained by using Edmunds&apos; method of removing carbon dioxide from the air and then adding a measured quantity. In any event, the test atmosphere was the same for all specimens in a test run. We agree with Mr. Anderson that the carbon dioxide content is important in the formation of a hygroscopic film on specimens. (2) We can imagine that there could be a concentration of solute atoms at the grain boundaries which would be so small that present methods would not detect it even if it exceeded the solubility limit of the alloy. There could be somewhat greater solubility at the grain boundaries for an interstitial solute. There is a possibility that phosphorus dissolves in this way but we believe that none of the other solutes studied does. In our present studies we hope to find out something about conditions at the grain boundaries of some of the systems mentioned in the paper. (3) Mr. Anderson points out that silicon brass, which has had a high temperature heat treatment followed by a quench. is highly resistant to stress-corrosion cracking. Although the test conditions used by Anderson* et al were different from our test conditions, it is noted that the silicon brasses which had not had the special heat treatment were less resistant to stress-corrosion cracking than copper containing approximately equal amounts of silicon. G. R. GOHN†—Nonferrous metallurgists and particularly, materials engineers, have been accustomed to thinking

Jan 1, 1950

By E. W. Davis

ABOUT a year ago several carloads of magnetite ore from New York state were sent to the Mines Experiment Station at the University of Minnesota for grinding and concentration tests. The flowsheet used minus ½ -in. ore as feed to a 3 by 3-ft. overflow cylindrical ball mill operating at 37 r.p.m. in closed ciruit with a vibrating screen. The screen oversize was returned to the mill for further grinding and the screen undersize was concentrated magnetically. Several different screens, between 8 and 35 mesh, were used and it was desired to determine the capacity of the ball mill operating in closed circuit with each screen. From earlier tests using this flowsheet and equipment, it was known that when comparatively coarse screens were used it was necessary to increase the grinding dilution in the mill beyond that ordinarily used when grinding in closed circuit with classifiers. It was also known that after the circulating load had passed about zoo per cent of the original feed it tended to increase rapidly in amount, and grinding conditions appeared to become unstable. These conditions may be peculiar to this small ball mill but they were very marked in this series of tests. If conditions were not right, the mill would suddenly "go dead," and it was found desirable to operate so that the occasional rattle of balls against the lining of the mill could be detected. As the test proceeded, it was found that the cure for almost any difficulty that developed in the grinding circuit was to add more water to the mill feed. To begin with, the mill was operated at pulp densities of from 60 to 65 per cent solids but gradually it was found that with higher dilutions grinding conditions were more stable and the ball-mill power per ton of screen undersize decreased. Actually, the most satisfactory operating conditions were secured with a pulp density of about 40 per cent solids. The ore was hard but it was possible to grind ½ in. feed so that all would pass an 8-mesh screen with a power expenditure in the ball mill of less than 2 1/2 kw-hr. per ton and with a circulating load of less than 50 per cent. With so high a dilution in the feed to the mill, it was feared that steel wear would be very high. However, the mill was not noisy, and in order to find exactly the grinding conditions, a special test was made at the end of the main series of tests. After the mill had been in operation for several hours and grinding conditions had become balanced, the power to all the equipment was shut off at a given signal. The ball mill made about one revolution after the power was turned off, and just as soon as the mill stopped, a spout was placed at the discharge trunnion and all of the pulp that flowed out of the mill was caught in tanks. The manhole in the mill was then opened and the whole mill charge dumped into other tanks. Both of these products were weighed, dried, and weighed again. The balls were screened out and weighed, and the dry solids were sized. In this way it was possible to determine the nature of the pulp and the ore within the mill under actual grinding conditions.

Jan 1, 1945

By H. L. B. Gould, Jr. Wenny D. H.

TO date there has been but limited interest in alloys of 80 to 95 pct Co and Fe with or without other additions. In 1932, S. R. Williams&apos; reported practically zero magnetostriction for the 90 pct Co-10 pct Fe alloy. This same composition was used for pole pieces to control the magnetic field in magnetrons operating at high temperatures.&apos; In 1947, a 90 pct Co, 9.5 pct Fe, and 0.5 pct Mn composition was investigated3 for use in ballast lamps because of its high temperature coefficient of resistance. Recently, as part of a survey of ductile and malleable magnetic alloys capable of being processed to thin gages for possible applications in memory devices, the high Co-Fe alloys have been re-examined to determine their fabricating and magnetic characteristics. Alloys from 80 up to 95 pct Co and Fe with and without additions such as vanadium were prepared. In general these all had excellent ductility and malleability. Wire was drawn to thin gages without difficulty and fine hard-drawn wires flattened to 2) The phenomenon may have potential in estimating the carbon content of molybdenum. A given solution-treating temperature and cooling rate could perhaps be calibrated so that the area fraction of surface covered by carbide could be interpreted in terms of carbon concentration. By segregating to the surface, a big "magnification" of the carbon content is obtained, which should make the method cheap, direct, and sensitive and, therefore, perhaps of interest to the molybdenum industry. This work was conducted at Battelle Memorial Institute. Financial support by the Aeronautical Systems Division, United States Air Force, under Contract No. AF 33(657)-7376, is gratefully acknowledged, and the writer is thankful for the experimental assistance of Miss Marjorie Cantin. ribbon without splitting. Similarly, strip was cold-rolled as much as 99.75 pct reduction to a 0.25 mil thickness without intermediate anneals. Samples of round and flat wire and foil, in the severely cold-worked and annealed states, were checked for magnetic characteristics. The alloys exhibited widely divergent magnetic characteristics depending on the processing and heat-treating procedures used in preparing the samples. Direct-current hysteresis loops showing the different magnetic characteristics of 90 pct Co, 9.5 pct Fe, and 0.5 pct Mn alloys are shown in Figs. 1 to 8 inclusive, while Figs. 9 and 10 show the loops for an alloy of 82 pct Co, 11.75 pct Fe, 5.6 pct V, and 0.65 pct Mn. Figs. 1 and 2 show the high remanence and exceedingly square-loop characteristics of the hard-drawn wire and ribbon roll flattened therefrom. With the change in processing from roll flattening to flattening by drawing through flat diamond dies the resultant change in texture is accompanied by the drastic change in the shape of the loop as shown in Fig. 3. This skewed loop on annealing reverts to a more normal loop as shown in Fig. 8. The most unique loops are obtained with flat rolled strip. These are shown in Figs. 4 and 5. In the case of the hard-rolled material, Fig. 4, there is little change in induction until the magnetizing force reaches 50 oe. From 50 to 60 oe there is a sharp increase in induction to over 15,000 gauss, which for all practical purposes is saturation. The induction remains at a constant value while the magnetizing force decreases to 40 oe. At this point the

Jan 1, 1965

By W. A. Backofen

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

Jan 1, 1952

By K. P. Gupta

In ternary systems containing silicon and transition elements, silicon was found to stabilize the a phase.1 At 1000°C a broad a-phase region was found in the Cr-Mn-Si system,1 which extends very close to the Mn-Si binary line (within about 3 at. pct Cr). Later investigation showed that, if chromium was replaced by small amounts (3 to 5 at. pct) of v,1 Ti, Nb, Ta, Mo, or w,1 the a phase or the R phase was again stabilized. Whether stabilization of complex crystal structures is possible by small additions of iron, cobalt, or nickel to Mn-Si is not known. Investigation of the Co-Mn-Si system4 shows the presence of several ternary phases, but at cobalt concentrations higher than 10 at. pct. In the present work the ternary systems Fe-Mn-Si and Co-Mn-Si were investigated at low iron and cobalt concentrations (< 7 at. pct Fe or Co) in search of phases of complex crystal structure. Experimental Procedure. The alloys were pre-pared by induction melting Co (99.8 pct), Si (99.9 pct), electrolytic Fe (99.88 pct), and Mn (99.9 pct) in recrystallized alumina crucibles under an inert atmosphere of argon gas. The alloy specimens were wrapped in molybdenum foil, sealed in argon-filled (at 1/2 atm) silica capsules and annealed for 72 hr at 1000" 1°C, and water-quenched. The use of argon-filled capsules was found to reduce the losses during annealing and the molybdenum foil prevented reaction of the manganese with silica. The total weight loss due to annealing and melting was found to be less than 1 pct for each alloy. The alloys were not analyzed chemically. A part of each annealed specimen was polished and examined metal-lographically using etching solutions, a) 0.1 to 0.5 pct oxalic acid solution in water, or b) 0.5 pct HNOs in methyl alcohol. Even though the etching solutions were quite dilute, the specimens were heavily etched and stained if the etching time exceeded more than 5 sec. Etching times found suitable were usually 1 to 3 sec. For X-ray diffraction work, a part of each annealed specimen was powdered by crushing after the exposed surface was ground off. X-ray diffraction patterns were taken with powder specimens using a 20-cm-diam asymmetrical focusing camera and Fe K radiation. These powder patterns were found quite satisfactory for the purpose of phase identification. However, X-ray diffraction patterns of single-phase alloy powder specimens were also taken using a Siemens diffractometer and filtered Cr-Ka radiation for greater resolution of the diffraction lines. Results and Discussion. In the Fe-Mn-Si system a new ternary phase was found at 1000°C between the p manganese and the MnsSi phase regions. The approximate phase relationships in this region of the 1000°C isothermal section are shown in Fig. 1. The new ternary phase, designated as the K phase, was found to occupy a narrow region about 1 at. pct in width and extending from Fee.oMn74.5Silg.5 to Fe.Mn.Silg.. At the high-iron content region, the K phase was found in equilibrium with the p manganese and the MnsSi phases but, at the low-iron content end of the K-phase region, the phases in equilibrium with the K phase were the p manganese phase, the MnsSi phase, and another new phase, designated in Fig. 1 as the v phase. The v

Jan 1, 1964

By H. W. R. Wardlaw

This paper shows how the cost of the drilling operation per 100-ft drilled can be related directly to bit weight, rotary speed and hydraulic horsepower variations. This enables optimum drilling conditions to be determined in a rapid and concise manner. The paper also shows how data for such calculations cun be obtained quickly and accurately by the "drill-off" method suggested by Lubinski. Examples are given to illustrate the principles and methods used. INTRODUCTION The problem of drilling oil wells at lowest cost and hazard needs little introduction, since it has been with us virtually from the earliest days of our industry. With better understanding of the effect of the various factors of bit weight, rotary speed and hydraulic jet action, however, the problem has recently taken on a more scientific aspect, and engineers or groups of engineers have been assigned to study many of the facets of this problem not immediately apparent to the general observer. Moreover, the availability of better equipment and materials has enabled certain practices to be adopted which were hitherto impractical or uneconomic. This has paved the way for further efforts to reduce footage costs, and so on. The improvements to be made in drilling technology and cost reduction are by no means exhausted, and we still frequently hear of new records being set and new materials and equipment becoming available. Some of the analytical methods used by the author to assist in promoting faster and more economic methods of drilling, particularly in Venezuela, form the basis for this descriptive study. STATEMENT OF THEORY AND DEFINITIONS In a highly competitive industry, it is no longer permissible to regard penetration rate as the sole criterion for drilling efficiency. Every new technique, however spectacular, must nowadays be viewed in the cold light of whether it will eventually lead to lower cost per foot drilled. In the exposition which follows, therefore, actual drilling rates will play only a secondary role, and attention will be focused on the more important aspect of cost per foot drilled. Changes in drilling factors such as weight and rotary speed will be studied in the light of how they directly affect the cost of operations. The advantage of this method is twofold—(1) cost increments are indicated directly; and (2) the relationships are, surprisingly enough, simpler than those relating to drilling rates. To achieve these advantages, it is necessary to introduce a new unit of measurement which, although unfamiliar, is readily understood. The unit in question will be referred to as the "actual drilling cost factor" and will be designated by the symbol h. The unit is defined as the number of rotating hours taken to penetrate 100 ft of formation. The unit can be obtained immediately from the actual drilling rate (r) in feet per hour; thus, This latter transformation is so easily effected that it may be convenient to use h as an international symbol for drilling cost, and to delay conversion to dollars, bolivars, pounds, etc, per foot until actually required (e.g., for fiscal reasons, etc.). In actual operations, h was found to vary in a relatively simple manner with increases in bit weight. The variation in h with rotary speed was found to be somewhat more complex. However, this also could be enormously simplified by introducing a further factor known as L or relative bit life. The factor L is also defined very simply by dividing 1,000 by the rotary speed (N) in revolutions per minute.

The Institute conducts jointly with the American Society of Civil Engineers, American Society of Mechanical Engineers and American Institute of Electrical Engineers, certain activities as listed below, and is joint owner with them of certain properties. United Engineering Trustees, Inc.* When Mr. Carnegie made his gift which made possible a home for the engineering societies, a separate corporation was organized to act as a holding company and to manage the common property. This was long known as the United Engineering Society but the name has now been changed to one which more nearly reflects the real function of the corporation. It holds title to the Engineering societies Building and to various funds placed in its charge and is managed by a Board of Trustees of which three are chosen by each of the four societies, American Institute of Mining and Metallurgical Engineers, American Society of Mechanical Engineers, American Institute of Electrical Engineers and American Society of Civil Engineers, which own equal and undivided interests in the property. The land and building cost two million dollars. The interest of each of the Founders societies, aside from especial trust funds, is now valued at $493,352. The A. I. M. E. trustees are Arthur S. Dwight, J. V. N. Dorr and H. A. Guess. George D. Barron will succeed Mr. Guess as trustee at the end of this year. The President of the Board is Francis Lee Stuart and the Secretary, Alfred D. Flinn. The Engineering Foundation The Engnieering Foundation was established in 1814 as a result of a gift of $200,000 made by Ambrose Swasey. It is intended not only "for the Furtherance of research" along broad lines but also "for the advancement of" a wide variety of other activities of benefit to engineering as need arises. The endowment fund, which now amounts to $630,000, is administered by the United Engineering Trustees, Inc. Through The Engineering Foundation board, on which the Institute is now represented by J. V. N. Dorr, John M. Callow and Galen H. Clevenger, the income of the endowment, approximately $28,000 a year, and funds contributed for special projects are appropriated for the purposes intended. H. C. Bellinger will succeed Mr. Callow on the board at the end of this year. Alfred D. Flinn is Secretary- and Director. Researches of wide interest in many lines have been aided by Engineering Foundation. . A grant from it to the Mining Methods Committee assisted in the preparation of Volume 72 of the Transactions. For several years the Foundation has aided in support of the study of Blast-furnacc Slags by R. 8. McCaffery at the University of Wisconsin, sponsored by the Institute. The Foundation has raised over $230,000 to support the Alloys of Iron Research endorsed by the Institute and George B. Water-house is serving as Chairman and Director of the Iron Alloys Committee which has been brought together to direct this work. The Foundation has also on recommendation of the Institute made a grant in aid of the studies of Mining and Strata being conducted at Columbia University by P. B. Bucky, which promise information of great usefulness relative to mine subsidence and support of ground. John Fritz Medal Board of Award The medal was established in 1902 and lias since, been awarded not oftener than annually by a hoard of sixteen members, four representatives each from the American Societies of Civil, Mining and Metallurgical, Mechanical, and Electrical Engineers.

Jan 1, 1930