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By L. T. Larson

The spectral reflectivity of zirconium in light of 441 to 668 nanometers (nm) wavelengths and air immersion has been determined. Bireflectance and apparent-angle -of-rotation measurements show zirconium to be optically isotropic when examined in light of approximately 484 nm wavelength. There is a direct relationship between bireflectance and the tilt of the basal pole of zirconium from the surface normal. This relationship allows the determination of the spatial orientation of the basal pole of an individual single crystal within a coarse-grained poly crystalline section to within± 2 to 3 deg for angles of basal pole tilt from 0 to 90 deg. In recent years considerable attention has been given to the quantitative determination of optical properties of opaque minerals by use of vertically incident, plane-polarized light. In particular, Cameron' and Cameron et a1.2 have developed criteria for the identification of a large number of anisotropic ore minerals based upon measurement of the apparent angle of rotation and the ellipticity or phase difference of the reflected light. It was shown by Larson and Pickle-simer3 that apparent-angle-of-rotation measurements may also be used to determine crystallographic orientations of grains of noncubic metals. In particular, it was shown that the basa.1 pole orientation in space of zirconium grains can be determined to ±3 deg for those grains with basal pole tilts of 10 to 90 deg from the plane of the section. Another, even more widely studied, optical property is reflectivity. cameron4 has commented upon measurement of the reflectance of plane-polarized, vertically incident light and Bowie and Taylor5 have made such measurements an integral part of their system of ore-mineral identification. Leow6 has reported on the spectral reflectivity of molybdenite and has used reflectivity values to calculate refractive indices and absorption coefficients. Cameron7 has made use of reflectivity values to ascertain aniso-tropic ore mineral symmetry and Piller and v. Gehlen8 have evaluated sources and importance of errors in reflectivity measurements as applied to calculation of optical constants. cambon9 has shown that reflectivity measurements using vertically incident, plane-polarized light are useful in the investigation of metals and in the identification of phases present in alloys. Bronson10 has made preliminary measurements on the optical anisotropy of beryIlium and Mott and Haines11 have published qualitative data on the intensity of light reflected from sections of bismuth, tin, and aluminum when these metals are microscopically examined under crossed polarizing plates. Koritnig12 has correlated the reflectivity of homogeneous solid solutions with their chemical compositions. From the above work and investigations in progress by this author, it is apparent that accurately determined values for the reflectance of vertically incident, plane-polarized monochromatic light from carefully polished surfaces of noncubic metals can prove useful in identification, composition determinations, and crystallographic orientation applications. Finally, reflectivity values, when measured in two media of differing refraction index and related to standards whose spectral reflectivities in these media are known, can be used to calculate optical constants such as refractive index and absorption coefficient. These constants may prove of use to those concerned with problems of electron band configuration. This paper reports the spectral reflectivity of zirconium measured in light of 441 to 668 nanometers (nm) wavelengths and air immersion. It also gives maximum bireflectance values for a prism section of zirconium in these wavelengths and shows how bire-flectance may be used to determine the crystallographic orientation of zirconium single crystals. Because of the lack of information on the reflectivities of the standards in oil immersion, no attempt is made to calculate the refractive indices or absorption coefficients although it is recognized that such values may be of fundamental importance. METHOD Single crystals of zirconium were cut by electro-discharge machining from a single-crystal rod grown from iodide bar by an electron-beam zone-melting process.13 The crystal sections were mounted in cold-setting epoxy resin and mechanically polished to a plane, uniform, bright surface. Each crystal was then chemically polished in a 26/26/43/5 mixture (by vol) of water, nitric, lactic, and hydrofluoric acids to remove the mechanically damaged and smeared surface layer. Final polish was obtained by electropolishing at 30 v in a bath of methyl alcohol and perchloric acid (98/2 by vol) at -70oc.14 Reflectivity measurements were made using a photometer system designed and developed at Oak Ridge National Laboratory and described in detail by Larson.15 Briefly, the reflectivity measuring system consists of a reflecting microscope; a double-beam, null-balancing photometer array; a mechanically driven microscope stage; and a direct X-Y readout of the reflectivity of the specimen relative to its orientation on the microscope stage. The measuring photometer receives its signal from the specimen through a slotted Wright occular placed on top of the photovisual head of the microscope. The reference photometer receives light through a flexible glass "light pipe" from a mirror in the reflecting system of the microscope. Monochromatic light is attained through use of interference filters (15-nm half-peak width pass bands) placed in front of a stabilized Vickers 12 v, 100 w, tungsten-filament, quartz-iodide lamp.

Jan 1, 1970

By R. B. Newcombe

Despite abnormal economic conditions and the unhealthy state of the petroleum industry, 1930 closed without any marked decline in total production of oil in the Middle Western States. The most accurate figures available would indicate for this district an output of close to 25,000,000 bbl. for 1930 as compared to 26,000,000 bbl. for 1929. This can be accounted for by the settled nature of a great many of the wells producing in this area and the favorable geographical position, which affords adequate refining and marketing facilities. The only new flush production field discovered in the area was the Legrande oil pool in southeastern Hart County in western Kentucky, where wells up to 1000 bbl. initial have been reported from a shallow depth. Important extensions have been found in a number of central Ohio fields, and activity in the central Michigan area resulted in new pools along the northwest trend of the Mt. Pleasant structure. These new districts, known as the Leaton and Vernon pools, have not yet reached the scope of the Mt. Pleasant field proper, and although the structure is similar, sand conditions are not strictly analogous. Wildcatting was retarded somewhat by the scarcity of market for oil and many important wells were shut down for several months. This has not shown such a profound effect on production as the reticence of operators to drill inside proven locations. The major companies have not been able to dispose of their oil and the smaller operating units are having trouble financing their projects. The result is that oil in sight is not being produced and output is suffering accordingly. Another important effect on production was the introduction of proration by the major crude purchasers and a voluntary shut-down by Kentucky operators. This step became necessary because of the glutting of lake port refineries with Mid-Continent oil, and was not fostered by regulating state bodies, as in the case of the southwestern states. Small refining units have sprung up to meet this situation in a number of instances but they have experienced some difficulty in disposing of their product because of "dumping" tactics from other quarters. New refinery outlets on the Great Lakes and new pipe line connections should tend to alleviate this difficulty during the coming year. The

Jan 1, 1931

NEW MEMBERS The following list comprises the names of those persons who became members during the period Sept. 10, 1916, to Oct. 10, 1916. BLOOMFIELD, EDWIN CHARLES, Min. Engr., 1012 Standard Bank Bldg., Vancouver, B. C., Canada. BRINGS, HENRY, Min. and Met. Engr., Chief Engr., and Geol., Mollet-Mesrine, 1212 Mills Bldg., El Paso, Texas. CHASE, MARCH F., Vice-Pres., Commercial Acid Co., 1906 Boatmens Bank Bldg., St. Louis, Mo. CUMMINGS, ALVIN M., Asst. Mine Supt., Witherbee, Sherman & Co., Inc., Mineville, Essex Co., N. Y. DOUGLASS, GEORGE M., Genl. Safety Inspector, Amer. Smelt. & Ref. Co. 120 Broadway, New Fork, N. Y. EMRICH, CLARENCE T., Chief Chemist, Old Dominion Copper Min. & Smelt. Co., Box 1163, Globe, Ariz. GARDANIER, SUTTER ALBERT, Assayer, Mgr., Douglas Assay Co., Douglas, Cochise Co., Ariz.

Jan 10, 1916

By Arthur S. Huey

AS the end of the collegiate year approaches, the problem of student employment again becomes acute. This subject divides itself into two phases: (1) employment prior to graduation and (2) employment following graduation. "Experience is the best teacher," according to the old adage, and the student needs all that he can get. He is afforded every opportunity to reap from his books the theories and principles of scientific and engineering practice, and occasionally he is privileged to make field trips to observe the practical side of the subject. But it is not enough for one to know the theory and to observe its application; it is also desirable for the student to get the feel of the tools during his training Such opportunities can only be afforded the student if the major companies cooperate with the universities in giving the student part-time and vacation work.

Jan 1, 1932

Establishment of a Bureau of Mineral Research at the Michigan College of Mining and Technology, initiated by the State of Michigan with legislation in 1951, is moving toward realization. The Michigan Legislature appropriated $24,000 to cover preliminary costs of plans and specifications for "engaging in a broad, widespread study of the beneficiation of lowgrade ores, of ore dressing, and all the problems of metallurgy that enter into such a program." Ralph C. Calder, of Detroit, who designed Michigan Tech's campus buildings, is preparing plans for the proposed Ores Research Building. Members of the college staff, Professors F. J. Tolonen, W. E. Keck, and Research Engineer Paul Jasberg are assisting in preliminary planning. C. Harry Benedict, retired chief metallurgist of Calumet and Hecla and a member of Michigan Tech's Board of Control, is assisting with technical details. Professor Nicholas Manderfield, head of the department of Mineral Dressing, was assigned to visit other research installations and suggest plans for the Bureau.

Jan 1, 1952

This discussion was prepared by members of the Phelps Dodge Corpn. staff who were designated to review the minutes. It is confidential but permission has been granted to distribute copies among those who attended the Conference. The minutes of the above conference contain numerous references to the plants and practices of Phelps Dodge Corporation. As many of these references are inaccurate, the following notes are made covering such points: Construction Magnesite Brick in Reverb. Arch (1) An.18" arch, 20 feet long, was built on one furnace with 5 feet on each side of magnesite brick, the center portion .being of silica brick. The furnace was put in operation February 13, 1930 and on April 23rd after 68.8 days' operation it was replaced due to failure of the silica brick forming the center of the arch. At this time, while the silica brick had completely gone, there was 14" of magnesite left. Bridgewall Tapping (2) Tapping matte through the burner wall was first tried at the Copper Queen Smelter in April, 1925. At that time, a copper casting with 1 ½ extra heavy pipes for water cooling cast in it, and having one taphole block was used. Later, on the other (old) furnaces, similar castings, but equipped with two tapholes, were used. We found with these furnaces that we could tap through the burner wall at the beginning of a campaign, but would subsequently have to go back to side wall tapping. This was the case until sometime in 1926. The new furnaces, that went in operation at the beginning of 1927, each had water. cooled castings with two tapholes. These have been used entirely and have been quite successful. Sometime after the furnaces were put into operation sidewall tapholes were put in, simply for the removal of any accumulation of matte that might be temporarily retained at the front end by bridges or dams in the furnace formed by overcharging locally.

Jan 1, 1930

By C. E. Lesher

THIS paper reports a study of the reactivity of 950°F and 1650°F cokes as measured by relative rates of reduction of iron oxides at temperatures up to 2200°F. Previous work cited shows general acceptance of the theory that reduction by carbon is a gaseous reaction, and that kind and character of carbon as well as particle size have measurable effect on the velocity of reaction. As will be shown, the data obtained in this study confirm those conclusions. The work was not designed to examine iron oxide reduction equilibrium, but if reaction velocity be defined as the speed with which "a reaction tends to approach conditions of equilibrium," the data here presented may be considered as a study of reaction rates, and the relative degree of reduction to metallic iron as the measure of reactivity. Three standardized combinations of Lake Superior brown iron ore with carbon were tested by similar procedures. One combination was a mechanical mixture of carefully sized high-temperature coke (1650°F) with the ore. The second was a mechanical mixture of the ore with Disco* obtained by carbonizing the identical coal at 950 °F. The third was an agglomerate prepared by carbonizing the coal and ore at 950°F, premixed in proportions to give as nearly as possible the same relative amounts of carbon and ore as the mechanical mixtures. This agglomerate, obtained by heating the finely divided ore (through 30 mesh) with coking coal through the plastic temperature range so as to form solid aggregates, gives a product in which the oxide particles are impregnated with, and intimately bound together with low-temperature coke. The agglomerate-—ore-Disco—was most active in oxide reduction; the mechanical mixtures of Disco and ore next in order, with coke the least reactive. General Discussion: Carbon exists in many forms and it is well known that the form or nature of the carbon used in reduction of oxides is related to the critical temperature of reduction. Sugar carbon, charcoal, and lampblack are forms of carbon that will reduce oxides at lower temperatures than high-temperature coke, and coke will, in turn, give a lower critical reduction temperature than graphite. There have been many investigations of this characteristic of carbons. Johnson' reported a difference of 130°F (70°C) in the critical reduction temperature of zinc oxide as between charcoal 1891 °F (1033°C) and Acheson graphite turnings 2021°F (1105°C) with zinc oxide. Bodenstein2 using charcoal and coke, found a difference of 138°F (77°C) comparing an experimental figure of 2066°F (1130°C) for coke and 1928°F (1053°C) for charcoal, in the reduction of zinc oxide. He concluded that this is very marked and observed that the "type of carbon merely raises or lowers the temperature at which rapid reaction takes place." Comparing the effectiveness of types of carbon in reduction of zinc oxide, it was found that a "brown coal coke" gave 97 pct zinc elimination at 1832°F (1000°C), as compared with 48 pct with "hard coal coke."' A wide range of metallic oxides was studied by Tammann and Sworykin,4 who found that the temperature at which decomposition of oxides begins depends on the nature of the carbon used. Carbon in the form of graphite, lampblack, and sugar carbon was investigated. Sugar charcoal will reduce Fe2O3 to Fe3O4 at 842°F (450°C) as compared with 1112°F (600°C) for coke, according to Meyer." Direct reduction of iron oxides by charcoal begins at 1382°F (750°C), but "first becomes intense" at 1652°F (900°C), whereas with coke, direct reduction begins at 1742°F (950°C), and "first becomes appreciable" at 2012°F (1100°C).6 he total reduction of the sample under certain conditions when heated in a current of CO with charcoal was about 100 pct for limonite and about 77 pct for magnetite. Using coke under the same conditions, the respective percentages were 75 and 47. In a study of processes for sponge iron7 by the Bureau of Mines, the conclusion was reached that a low-temperature char from noncoking subbituminous coal is the most satisfactory solid reducing agent. In a critical study of zinc smelting from a theoretical viewpoint Maier8 concluded that the reduction is by CO, that the reaction between ZnO and CO is intrinsically more rapid than the subsequent reduction of CO2 by C, which is limited by diffusion rates, which in part effectively limits the smelting process. Maier said that the operation is improved with the activity of the reducing carbon. An active carbon, he said, is one maintaining a low CO, content in the retort. Reactivity of Carbon: One form of carbon is more potent in reducing oxides than another. A carbon that reacts faster than another at a given temperature is said to be more reactive. Reactivity is measured by several methods, using carbon dioxide, air, or steam as reactants.9 ebastian and Mayers" have developed a method for the determination of absolute reaction rates between coke and oxygen by a study of ignition points under certain conditions. These and other investigators have established the relative reactivity of types of carbon. Lignite, charcoal, bituminous coal, cokes in the ascending order

Jan 1, 1951

By C. E. Lesher

THIS paper reports a study of the reactivity of 950°F and 1650°F cokes as measured by relative rates of reduction of iron oxides at temperatures up to 2200°F. Previous work cited shows general acceptance of the theory that reduction by carbon is a gaseous reaction, and that kind and character of carbon as well as particle size have measurable effect on the velocity of reaction. As will be shown, the data obtained in this study confirm those conclusions. The work was not designed to examine iron oxide reduction equilibrium, but if reaction velocity be defined as the speed with which "a reaction tends to approach conditions of equilibrium," the data here presented may be considered as a study of reaction rates, and the relative degree of reduction to metallic iron as the measure of reactivity. Three standardized combinations of Lake Superior brown iron ore with carbon were tested by similar procedures. One combination was a mechanical mixture of carefully sized high-temperature coke (1650°F) with the ore. The second was a mechanical mixture of the ore with Disco* obtained by carbonizing the identical coal at 950 °F. The third was an agglomerate prepared by carbonizing the coal and ore at 950°F, premixed in proportions to give as nearly as possible the same relative amounts of carbon and ore as the mechanical mixtures. This agglomerate, obtained by heating the finely divided ore (through 30 mesh) with coking coal through the plastic temperature range so as to form solid aggregates, gives a product in which the oxide particles are impregnated with, and intimately bound together with low-temperature coke. The agglomerate-—ore-Disco—was most active in oxide reduction; the mechanical mixtures of Disco and ore next in order, with coke the least reactive. General Discussion: Carbon exists in many forms and it is well known that the form or nature of the carbon used in reduction of oxides is related to the critical temperature of reduction. Sugar carbon, charcoal, and lampblack are forms of carbon that will reduce oxides at lower temperatures than high-temperature coke, and coke will, in turn, give a lower critical reduction temperature than graphite. There have been many investigations of this characteristic of carbons. Johnson' reported a difference of 130°F (70°C) in the critical reduction temperature of zinc oxide as between charcoal 1891 °F (1033°C) and Acheson graphite turnings 2021°F (1105°C) with zinc oxide. Bodenstein2 using charcoal and coke, found a difference of 138°F (77°C) comparing an experimental figure of 2066°F (1130°C) for coke and 1928°F (1053°C) for charcoal, in the reduction of zinc oxide. He concluded that this is very marked and observed that the "type of carbon merely raises or lowers the temperature at which rapid reaction takes place." Comparing the effectiveness of types of carbon in reduction of zinc oxide, it was found that a "brown coal coke" gave 97 pct zinc elimination at 1832°F (1000°C), as compared with 48 pct with "hard coal coke."' A wide range of metallic oxides was studied by Tammann and Sworykin,4 who found that the temperature at which decomposition of oxides begins depends on the nature of the carbon used. Carbon in the form of graphite, lampblack, and sugar carbon was investigated. Sugar charcoal will reduce Fe2O3 to Fe3O4 at 842°F (450°C) as compared with 1112°F (600°C) for coke, according to Meyer." Direct reduction of iron oxides by charcoal begins at 1382°F (750°C), but "first becomes intense" at 1652°F (900°C), whereas with coke, direct reduction begins at 1742°F (950°C), and "first becomes appreciable" at 2012°F (1100°C).6 he total reduction of the sample under certain conditions when heated in a current of CO with charcoal was about 100 pct for limonite and about 77 pct for magnetite. Using coke under the same conditions, the respective percentages were 75 and 47. In a study of processes for sponge iron7 by the Bureau of Mines, the conclusion was reached that a low-temperature char from noncoking subbituminous coal is the most satisfactory solid reducing agent. In a critical study of zinc smelting from a theoretical viewpoint Maier8 concluded that the reduction is by CO, that the reaction between ZnO and CO is intrinsically more rapid than the subsequent reduction of CO2 by C, which is limited by diffusion rates, which in part effectively limits the smelting process. Maier said that the operation is improved with the activity of the reducing carbon. An active carbon, he said, is one maintaining a low CO, content in the retort. Reactivity of Carbon: One form of carbon is more potent in reducing oxides than another. A carbon that reacts faster than another at a given temperature is said to be more reactive. Reactivity is measured by several methods, using carbon dioxide, air, or steam as reactants.9 ebastian and Mayers" have developed a method for the determination of absolute reaction rates between coke and oxygen by a study of ignition points under certain conditions. These and other investigators have established the relative reactivity of types of carbon. Lignite, charcoal, bituminous coal, cokes in the ascending order

Jan 1, 1951

By William B. Phillips

This paper was prepared at the request of Capt. A. F. Lucas, Chair man of the Institute's Committee on Petroleum and Gas; as a pre1iminary.discussion of the fuel oils which are used in the Southwest, giving their composition, uses, prices, etc. Should it afterward be found desirable, these observations may be extended over a larger area. In this connection, I suggest that samples of all kinds of fuel oils, including various tars, from all over the country, be collected and sent to some testing laboratory for examination. We would be glad to extend the facilities of the laboratory of the Bureau of Economic Geology and Technology, at the University of Texas, for this purpose, and to do the work free of all expenses. After such examinations are made and the results classified and studied, it would be possible to suggest specifications under which fuel oils should be purchased, and to arrive at some conclusions respecting the uniformity of such specifications, with due allowance for climatic and other more or less local conditions. While such specifications do not now depart from a common standard anything like as much as specifications for illuminating oils do, yet there are discrepancies which should not exist. Some of these discrepancies are of lessening importance, due to the pronounced tendency to distill every crude oil that can be distilled with profit, and to send residues into the market for fuel oil. Residues from the refineries are of a more uniform chemical composition and physical nature than many of the crude oils that go direct into the fuel market. The lower flash-point oils are disappearing from the fuel trade and in place of them we are getting oils that do not flash below 220" F., nor burn under 320" F. In the Southwest, it has not been long since we had fuel oils that flashed as low as 110" F., and the average flash point over a considerable period was 151" F. Now we are using oil that flashes at about 30" lower than the former burning point, which was 258" F. In other words, the flash point has risen, on the average, 100"; and the burning point about 75".

Jan 1, 1915

By R. M. Hudson

Equilibrium constants have been determined for the jeaction C (in steel) + H2O = CO + H2 as a function of carbon content (0.013 to 0.74 ujt pct) and temperature (1200° to 1800°F) by using a flow system in which the water-vapor content of various gas mixtures containing hydrogen, carbon monoxide, and nitrogen was systematically controlled. The equilibrium partial-pressure ratio K1 = PcoPH2/PH2O was obtained for two low-carbon steels and four Fe-C binaries from a series of runs made at each temperature. By comparison of Ki with the analogous ratio for the reaction C (graphite) + H2O = CO + H2, the activity of carbon in steel (ac) was comDuted for each temperature and carbon content studied. From these data values of the equilibrium constants for two other carburization-decarburiza-tion reactions of importance were estimated. The chemical compositions of the two steels and four Fe-C binaries used are given in Table I. Specimens of Steel E were cut from a 0.035-in.-thick commercially box-annealed and temper-rolled lot of a low-carbon low-metalloid steel. Steel F was a commercially hot-rolled rimmed steel that was cold-reduced at the Laboratory to a 0.059-in. thickness. Fe-C binaries A, B, C, and D were vacuum-melted and poured, hot-rolled, pickled, and cold-reduced at the Laboratory to furnish specimens 0.035 in. thick. Sheet specimens were cut from all lots to approximately 3/4 by 3 in. by gage and were vapor-degreased with trichlo-roethylene and weighed before heat treatment. Heat treatments were carried out in a hinged-top Hevi-Duty electric furnace with a Vycor-glass tube. When the furnace was at the desired

Jan 1, 1965

By D. G. Westlake

Resistance was measured as a function of temperature, 77° to 350°K,for niobium with hydrogen concentrations up to 3.76 at. pct. Cooling curves exhibited a discontinuity in slope that was attributed to the initiation of hydride formation. A thermal hysteresis was explained in terms of diffusion and the effects of mechanical constraint on nucleation and growth. The heat of solution of hydrogen in saturated Nb-H solid solution was 2. 737 * 0.045 kcal per g-atom, including an unknown stress contribution. The critical ternperatures for hydride formation during cooling and for embrittlement are correlated but not coincident. This, too, has been explained in terms of mechanical constraint and stress-itlduced tratzsfomtation. Nb-H alloys undergo a ductile-brittle transition with decreasing temperature.'-3 Similar behavior has been noted for v-H.1,5 For the latter system, there is evi-dence6 suggesting coincidence of the temperature of minimum ductility and the critical temperature T, for initiation of metal hydride precipitation during cooling. A decrease in ductility due to the presence of brittle hydride particles is readily explainable. The fact that ductility begins to decrease at some temperature higher than T,4,5 has led us6 to suggest that precipitation may be strain-induced locally during tensile testing. Wood and Daniels' have reported that a plot of temperatures for 10 pct reduction in ductility vs hydrogen concentration in niobium is not coincident with, but parallels, the solvus.7,8 They believe this indicates a correlation of precipitation and embrittlement. Unfortunately, the two reported solvuses 7,8 to which Wood and Daniels refer are not in agreement with each other. Furthermore, neither solvus was determined experimentally: each was a plot of calculated solubilities. Thus. neither is highly dependable for determining whether embrittlement coincides with initiation of hydride precipitation. Longson 9 studied phase relations in the Nb-H system between 77° and 473°K by dilatometry. Comparison with metallographic observations convinced him that discontinuities in the slopes of his dilatometric plots were coincident with the initiation of hydride precipitation. Plotting the logarithm of the hydrogen concentration vs the reciprocal of the temperature at which precipitation was initiated during cooling, he obtained a straight line shown in Fig. 1. Walter and chandler,'' using X-ray techniques to detect the for mation of a second phase? have obtained three experimental points in the temperature range 295° to 338°K which fall within Longson's experimental error for this plot. A similar plotg of temperatures at which dissolution was completed during heating was a parallel line shifted toward higher temperatures. A straight-line plot was obtained, also, for the temperatures of the ductile-brittle transitions,9 but it was shifted toward still higher temperatures. Longson calculated an activation energy of 2.980 * 0.300 kcal per mole for the hydrogen embrittlement mechanism, compared with 3.180 * 0.400 kcal per mole for hydride formation. Despite this agreement, he concluded, "It seems unlikely that embrittlement results from hydride formation..." because hydrogen embrittlement was observed at temperatures above the solvus. It is our contention that embrittlement is correlated with precipitation of the hydride.6 Because only Longson has investigated Nb-H phase relations at sub-ambient temperatures, we deemed it advisable to re-determine the temperature dependence of the solubility using the resistometric technique already proven successful for the V-H system.6 Coincidence of our solvus with temperatures for embrittlement would

Jan 1, 1970

By B. C. Allen

Liquid surface tensions of copper and 18 Group IV-A to VIII transition metals (Ti, Zr, Hf, V, Cb, Ta, Mo, W, Re, Ru, Rh, Pd, Os, Ir, Pt, Fe, Ni. Co) have been measured by the static pendant-drop and dynamic drop-weight methods on the same rod sample. The drops were formed by electron-bombardment heating in high vacuum. Application of necessary corrections enabled determination of surface tensions to k2 pct and agreement between methods to * 1 to 4 pct for all the metals studied. Evidence is presented that the liquid surface was well screened by metal vapor, suggesting negligible adsorption of gaseous impurities and that the surface tensions measured are characteristic of the metals involved. Correlations between liquid surface tension and melting point, molar volume, heat of vaporization, and atomic number are presented and discussed. Temperature coefficients of surface tension were calculated using Eötvös' law. SURFACE tension and interface energies of metals are the result of incomplete atomic coordination resulting in a force perpendicular to the boundary, tending to minimize its area. These energies are important in many phases of metallurgy, including microstructure, sintering, joining, electronic emission, and lubrication, which in turn affect many physical and mechanical properties of metals. Liquid surface tension refers to the interface between the liquid and its own vapor or nonreactive atmosphere, and is considered a physical property of the liquid. Since equilibrium shapes can be readily obtained with liquids, the units of surface tension (force per length) and interface energy (energy per area) are interchangeable. Thermo-dynamically, the surface tension ?LV is given by the change in free energy F with surface area A at constant pressure P, temperature T, and composition N: for commercially important refractory metals, vanadium, columbium, tantalum,13,14 molybdenum,14 and tungsten,l5 and none for the rare platinum-group metals and rhenium. Measuring the surface tensions of transition metals is difficult because of their high reactivity and melting points. Of the many techniques available,16-18 the pendant-drop 19-21 and drop-weight methods17,22 are considered superior because they can be modified to eliminate persistent sources of contamination such as supports and capillaries necessary in the popular sessile drop, capillary rise, and maximum-bubble-pressure techniques. The necessary modification is to melt a drop on the tip of a vertical rod, which provides support through a solid of the same composition.13,15 The object of the work was to study the surface-tension behavior of copper and transition metals, having reasonably low vapor pressures. Liquid surface tension of each pure metal was systematically determined by using a combination of the static pendant-drop and dynamic drop-weight methods on the same rod. Liquid drops were formed by electron-bombardment heating in high vacuum. EXPERIMENTAL WORK As indicated in Table I, the metals studied were high purity and generally were obtained in rod form. The exceptions were titanium and zirconium, which were machined from crystal bars, and molybdenum (tot 11, osmium, and ruthenium, which were sintered and arc cast into rods. All the metals were ground or swaged to desired sizes between 1- and 7-mm diam, and centerless ground round and smooth to a finish better than 50 µ in., rms. Each rod was thoroughly cleaned with steel wool, degreased, acid etched, and dried. In a typical run, the rod was vertically clamped in a modified floating-zone electron-bombardment furnace designed after Calverley23 and Carlson.24 The specimen was outgassed and maintained positive at several kilovolts in a dynamic vacuum of 10-5 to 10-7 mm. The bottom end was enclosed by a tantalum pillbox and heated by electrons emitted from a hot concentric tungsten filament mounted on a movable bracket. The bombardment power was slowly raised until melting was observed. Power requirements ranged from 30 w for copper to 1300 w for 4-mm tungsten. The stabilized and out-gassed drop of near-maximum size was photographed at 4. 1X on panchromatic film at desired time inter-

Jan 1, 1963

ALABAMA Anniston.-Bretz, J. A. Carrington, F. G. Gerber, A. B. Klugh, B. G. Semple, R. A. Ashland.-Barton, .J. Bessemer.-Abbott, C. E'. Ball, T. L. Beaver, J. J. Ferguson, V. Salmon, H. S. Sehaber, C. F. Whatley, W. J.

Jan 1, 1923

THE metal iron has physical and chemical properties which are somewhat different from those of steels, but a knowledge of the pure metal is a useful starting point in studying the behavior of steels. Solid iron exists in two different crystalline forms, called alpha (a) and gamma (?) iron, the former being the ordinary form at room temperature. When heated above the "A2 point," 1400°F. (760°C.), the metal becomes non-magnetic, and at the "As point," 1670°F. (910°C.), it undergoes a change in crystalline form to become gamma iron. In the range 1400 to 1670°F., it is sometimes called beta (0) iron to distinguish it from the magnetic alpha, but the two are identical in crystal structure. When gamma iron is further heated to 2550°F. (1400°C.), it changes into delta (d) iron, which is identical with beta or non-magnetic alpha iron. Pure iron melts (in a hydrogen atmosphere) at 2795°F. (1535°C.); the melting point is generally lowered by alloys or impurities. PROPERTIES OF IRON AT HIGH TEMPERATURES Many of the properties of iron undergo abrupt changes at the transition temperatures. (1) For example, in heating through the As point a sudden shrinkage in volume occurs. Similarly, melting is attended by sharp physical changes such as an increase in volume. Table 27 contains a summary of the measured physical properties of pure iron at several temperatures. Usually the properties change smoothly within the range of stability of a given form, but this is not always the case. For example, the specific heat reaches a sharp maximum at the A2 point although no transformation occurs. Solvent Powers of Liquid Iron. Liquid iron is capable of dissolving most of the other metals and many nonmetallic elements as well. Of the metals which are liquid at the melting point of iron only lead, silver, and bismuth refuse to dissolve to an appreciable extent. The non-metals presumably dissolve by virtue of the formation of an iron compound; for example, sulphur is thought to dissolve as the compound FeS. However, there is no satisfactory method of proving that this

Jan 1, 1944

By George G. Binder Jr., James W. Lacey, Arthur L. Draper

An experimental investigation of miscible fluid displacement has been made in linear porous media under highly adverse mobility ratio conditions. Various refined oils were displaced at field rates by liquid propane in both horizontal and vertical models 9 to 36 ft in length. In horizontal tests, mixed zones or transition zones form between the two liquids early in the displace-lents. Initially, the zones grow rapidly. III 2-in. diameter models, the mixed regions become nearly stable zones from 6- to 20-ft long. From then on these quasi-stable zones apparently grow only by molecular diffusion. The lenghts of the quasi-stable zones appear to be almost independent of the core material in which displacement;; are made and increase with increasing rates of injection and oil/solvent viscosity ratios. The lengths of the quasi-stable zones. measured in 2-in. diameter models at viscosity ratios and injection rates anticipated in the field indicate that essentially piston-like displacements of oil by solvent would occur. However, the mixed zone lengths increase markedly as the model diameter increases. In vertical displacements controlled by gravity drainage, only short trans-sition zones form. The entire lenghts of these zones can be accounted for by molecular diffusion. Therefore, in reservoirs having characteristics allowing a high degree of gravity drainage, nearly complete oil recovery should be attainable by miscible fluid displacement. INTRODUCTION The oil industry is faced with an ever increasing cost for finding new oil reservoirs. This, coupled with the fact that conventional methods of oil recovery usually leave from 1 to 3 bbl of oil in the ground for every barrel produced, has aroused considerable interest in developing more efficient methods. An integral part of the mechanism of many of these new methods of recovery is a miscible fluid displacement in which oil is displaced by a much less viscous materiai such as liquid propane. A numher of irlvestigators have explored the mechanics of miscible fluid displace-ment,'.2.1.'."." but in the experiments reported many of the important factors have been varied only over a limited range far removed from norma1 oilfield values. This paper presents the results of an experimental study of oil displacement by liquid propane at field rates from linear, natural-sandstone models of various sizes. Both horizontal and vertical flow tests were made. EXPERIMENTAL APPARATUS AND PROCEDURE Refined oils with viscosities varying over a wide range were displaced at several rates by liquid Propane from both horizontal and vertical flow systems. The behavior of the displacement was observed by propane-oil analyses of the effluent and, when possible, by differential pressure measurements along the cores. A schematic flow diagram of the apParatus used to conduct the experirents is shown in Fig. 1. The cores used in the tests were 9-ft lengths cut from natural consolidated sandstone and turned to the desired diameter. These were cast in steel tubing with a low melting point (160°F) alloy which expands on solidification. Flanges welded to the ends of the steel pipes permitted sealing the ends or butting one core to another. Pressure seals were maintained with O-rings. The cores were cleaned by flushing

With a total value to date of well over $200,000.000.00 for its ore production, the Tintic mining district, which is about 100 miles southwest of Salt Lake City, ranks as one of the three main ore producing areas of Utah. In it are located the biggest silver mines of the country, silver having been the chief metal produced in the camp since its start. Tintic's silver production to date has a total value of over $1 00,000,000, approximately half of the value of the camp's ore production, the balance being roughly divided among lead, gold and copper. Discovery of the camp was made in the late sixties. Lack of transportation and ore reduction facilities delayed extensive development of the area for nearly a decade. In recent years Tintic's ore production has ranged from 350,000 to 400,000 tons annually. In 1924 the camp produced one-eighth of the silver produced in the nation with an output of 7,729,700 ounces. Its lead production was 77,765,000 pounds and its gold production 26,285 ounces.

Jan 1, 1925

By William Mikulas

LITTLE work has been done in the field of the nickel-tin binary system. The complete diagram has been investigated on two occasions, but the results are in very poor agreement. The structure of a compound NiSn, and the solubility of tin in nickel have been determined by X-ray methods. Several investigations have been made of the liquidus curve, and the compositions of the eutectics have been determined. A study of the literature, however, shows that there is no satisfactory agreement between the data presented in the various papers. The present investigation was undertaken in an attempt to determine the equilibrium conditions, and to correlate X-ray with metallographic data. The equilibrium diagram was determined by thermal and metallo-graphic means, and the solubility of tin in nickel further investigated with X-rays. Powder diagrams were made of the intermetallic com-pounds, and three of the structures were partly determined. No attempt was made to determine the range of homogeneity of the inter-metallic compounds.

Jan 1, 1937

By Murray F. Hawkins

Horner1 and van Everdingen8 ave shown that the pressure drop within the wellbore, as a result of having produced the well at a constant rate q for time t, where t is sufficiently large, is: van Everdingen observed that better agreement between theory and well performance can be obtained if, instead of assuming the permeability is kc everywhere about the well, it is assumed the permeability near the well-bore is substantially reduced as a result of drilling, completion and/or production practices. In order to account for the additional pressure drop he introduced the dimensionless quantity S, the skin effect factor, so that Eq. 1 becomes: Eq. 2 might have also been obtained as follows. Assume a zone of altered permeability k, exists about the well out to a radius r and beyond that the unaltered, external permeability k. The additional pressure drop required to overcome this skin of reduced permeability may be calculated with sufficient accuracy using the incompressible flow equation; for Browns-combe and Collins1 have shown almost no difference between compressible and incompressible steady-state flow, in the vicinity of the wellbore, and the small volume of fluid in the vicinity of the wellbore makes unsteady-state mechanics unnecessary. Then. The sign of this skin pressure drop will be positive or negative depending upon whether the altered permeability k, is smaller or larger, respectively, than the external permeability k... Adding the pressure drop of Eq. 3 to Eq. 1 to find the total pressure drop: Comparing Eq. 4 with Eq. 3 it is seen that the skin effect may be defined by: be determined from pressure build-up tests1,3,4,5,6,7,8 The average permeability kavg including the altered and external permeabilities, can be determined from PI tests, and may be defined approximately on the basis of steady-state flow, as was done by Thomas' in defining the damage factor, by: The productivity ratio is the ratio of the average to the external permeability, kavg/ke or This equation shows that the productivity ratio and the skin effect are not uniquely related, because of the uncertainty in the drainage radius, and also, in many instances, the wellbore radius. Fortunately, they enter in the logarithm. The curves of Fig. I are plots of Eq. 8 for values from 100 to 50,000. The points represent the skin effects and corresponding productivity ratios from a large number of well tests, taken from Fig. 15 of Ref. 5 or Fig. 13 of Ref. 9. While some of the data

Jan 1, 1957

By AIME AIME

PRESIDENT Edwin Ludlow and Secretary Bradley Stoughton made their first-trip of the year 1921 to visit Local Sections of the Institute, and talk over Institute interests and policies, during the early part of April. The main purpose of the trip, as usual, was to bring back to headquarters suggestions or comments on the Institute's work on the part of, members. The trip was made a brief, one by the necessity of remaining in New Fork until Apr. 1, and of the attendance of President Ludlow at a meeting of American Engineering Council and. the organization of a Philadelphia Section of the Institute in Philadelphia on Apr. 16.

Jan 1, 1921

(Under this heading will be published notes sent to the Secretary of the Institute by members or other persons introduced by members) Member, Graduate Colorado School of Mines. Four years' experience in West and Northwest. Two years with American Smelting and Refining Co. Wishes to join field party on geological work, mining or areal, where opportunity will be given to be of direct assistance to chief of party in solution of field problems. Age, 26. Unmarried. At liberty June 1. No. 342. Member, technical graduate, aged 30, with' 7 years' experience in concentrating and mining, desires a position of authority with reliable company. At present employed. No. 343. Member. Ambitious, energetic, tactful engineer, college graduate, married, aged 30, desires location with a large coal mining organization. Seven years with present employers -n middle west; has had broad experience in the past eight years on examination, development and construction; successful record in handling men. Position must carry responsible work and a future. Will go anywhere for proper opportunity. Exceptional references as to reliability, character and capacity for work. No. 344.

Jan 3, 1917