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By W. F. Holbrook

IN a previous paper1 a method for the measurement of the comparative desulphurizing power of slags was described and data were presented covering the range of likely slags containing up to 10 per cent MgO In the present work the range is extended to include slags containing up to 20 per cent MgO, and the effect of temperature on 5 per cent and 15 pen cent MgO slags over the range 1475° to 1525° C is included The method used was that described in the previous paper except that some of the temperature measurements were made with a noble-metal thermocouple instead of a tungsten-graphite thermocouple Twelve-gram charges of 0 8 per cent sulphur-metal and 5-gram charge-, of slag were subjected to heating for 30 nun at a prescribed temperature The charges were analyzed for sulphur content For purposes of comparison, desulphurizing power is defined as the ratio of the percentage of sulphur found in the slag to that found in the metal Six slag and metal charges were made coincidentally in 5/8-in holes in a section of an electrode graphite rod One slag and metal charge was used as a control by means of which adjustment in the desulphurization value could be made for small variations in temperature and other factors For convenient presentation of the data, the slags are arranged in groups in each of which one of the four main slag components is constant Thus, the 15 per cent MgO slags are presented separately from those containing 20 per cent MgO SLAGS WITH MAGNESIUM OXIDE CONSTANT 15 Per cent MgO -The data on slags containing 15 per cent MgO cover a composition range of 24 to 50 per cent SI02, 5 to 27 per cent A1203 and 24 to 53 per cent CaO Variation in composition has been in steps of 2 per cent over much of the area Because the change in desulphurization power is generally gradual with gradual change in composition, certain sections have been covered m steps of 4I per cent and even

Jan 1, 1938

By NEWTON B. KNOX

CHILEAN mining in the public mind is rightly associated with copper. Chuquicamata with its great hill of copper-bearing granodiorite as well as Sewell and Potrerillos with mineralized volcanic necks together can supply a good proportion of the world's normal necessities of that metal. Chile is an extremely long and narrow country, averaging only 109 miles wide. Its eastern frontier is the Andes and it is on the western slopes of these mountains that the great copper deposits have been discovered. West of the Andes a great longitudinal depres sion has permitted accumulation of nitrates and other soluble salts in the arid north; in the north center it is hidden by a series of cross ranges, but in the center a moderate rainfall makes it the country's most important agricultural region. In the south this depression is drowned and gives rise to a series of straits and fiords. This enormous cleft in the earth's crust is separated from the sea by a coast range of moderate elevation which in the south is represented by a series of islands and mushroom-shaped peninsulas

Jan 1, 1945

By D. B. Carson, D. L. Katz

Natural gases under pressure form crystalline hydrates with water. Experimental data are reported on four-phase equilibrium for the methane-propane-water, methanc-pentane-water, and methane-hexane-water systems. Temperatures and pressures for equilibrium between gas, water-rich liquid, hydrocarbon-rich liquid, and hydrate were measured, as well as the percentages of methane and propane in the hydrate. The data indicate that natural gas hydrate behaves as a solid solution and that pentanes and heavier hydrocarbons do not enter into the solid phase. Vapor-solid equilibrium constants are presented that permit the approximation of the conditions for hydrate formation, from the composition of a gas. Introduction Natural gas hydrates have been the object of considerable research in recent years, because of the trouble they have caused in the natural-gas and natural-gasoline industries. Natural gas hydrates are white crystalline compounds of water and gas, which, under pressure, exist at temperatures considerably above the freezing point of water. Because of the relatively high temperatures at which the hydrates exist, they become a nuisance in high-pressure gas operations where water is present, since their formation causes partial or complete plugging of valves and pipes. From a practical standpoint, the trouble incident to hydrate formation has been solved by dehydration of the gas before it enters the plant or pipe line, or by other remedial measures. Extensive work on gas hydrates in the latter part of the nineteenth century, by Villardl and others, gave data on methane hydrate and on ethane hydrate. Schroeder summarized these theoretical studies2 Hammerschmidt3 introduced the information on gas hydrates to the gas industry and Dcaton and Frost4-6 gathered a considerable number of data on the behavior of natural gas hydrates. Recent papers7,8 have extended both the data and the theory of these hydrates. At present, data are available on tem-peraturcs and pressures of hydrate forma. tion for pure methane, ethane, propane, n-butane, methane-ethane mixtures, meth-ane-propane mixtures, methane-butane mixtures, and some Is natural gases, all- in the Presence of excess water. However, up to the Present time no method has been available for predicting the temperature at given pressures or the pressure at given at at which natural gases will form hydrates if hydrates with water. 'This Paper Presents data on the methane-propane-water, methane-pentane-water and methane-hex-""e water systems in four phases, one of which is the hydrate. he application of the phase rule to the methane-~ro~ane-water data Proves that hydrates behave as solid solutions. The data of this paper and those in the literature were used to develop vapor-solid. equilibrium constants,8 which permit prediction of conditions of hydrate formation from the analysis of a natural gas.

Jan 1, 1942

By D. B. Carson, D. L. Katz

Natural gases under pressure form crystalline hydrates with water. Experimental data are reported on four-phase equilibrium for the methane-propane-water, methanc-pentane-water, and methane-hexane-water systems. Temperatures and pressures for equilibrium between gas, water-rich liquid, hydrocarbon-rich liquid, and hydrate were measured, as well as the percentages of methane and propane in the hydrate. The data indicate that natural gas hydrate behaves as a solid solution and that pentanes and heavier hydrocarbons do not enter into the solid phase. Vapor-solid equilibrium constants are presented that permit the approximation of the conditions for hydrate formation, from the composition of a gas. Introduction Natural gas hydrates have been the object of considerable research in recent years, because of the trouble they have caused in the natural-gas and natural-gasoline industries. Natural gas hydrates are white crystalline compounds of water and gas, which, under pressure, exist at temperatures considerably above the freezing point of water. Because of the relatively high temperatures at which the hydrates exist, they become a nuisance in high-pressure gas operations where water is present, since their formation causes partial or complete plugging of valves and pipes. From a practical standpoint, the trouble incident to hydrate formation has been solved by dehydration of the gas before it enters the plant or pipe line, or by other remedial measures. Extensive work on gas hydrates in the latter part of the nineteenth century, by Villardl and others, gave data on methane hydrate and on ethane hydrate. Schroeder summarized these theoretical studies2 Hammerschmidt3 introduced the information on gas hydrates to the gas industry and Dcaton and Frost4-6 gathered a considerable number of data on the behavior of natural gas hydrates. Recent papers7,8 have extended both the data and the theory of these hydrates. At present, data are available on tem-peraturcs and pressures of hydrate forma. tion for pure methane, ethane, propane, n-butane, methane-ethane mixtures, meth-ane-propane mixtures, methane-butane mixtures, and some Is natural gases, all- in the Presence of excess water. However, up to the Present time no method has been available for predicting the temperature at given pressures or the pressure at given at at which natural gases will form hydrates if hydrates with water. 'This Paper Presents data on the methane-propane-water, methane-pentane-water and methane-hex-""e water systems in four phases, one of which is the hydrate. he application of the phase rule to the methane-~ro~ane-water data Proves that hydrates behave as solid solutions. The data of this paper and those in the literature were used to develop vapor-solid. equilibrium constants,8 which permit prediction of conditions of hydrate formation from the analysis of a natural gas.

Jan 1, 1942

By Harry W. Antes

The density changes that occurred on annealing cold-worked poly crystalline molybdenum, over the temperature range of 870" to 1630 SC, were determined. Increases in density were observed for recovery and the beginning of recrystallization. An initial decrease in density was observed during re-crystallization. A second decrease in density was observed after recrystallization was completed, as the microstructure changed from columnar grains to equiaxed gvains Both decreases in density were associated with an increase in gain boundary area to volume ratio. The second decrease in density was observed in the annealing range that immediately precedes secondary recrystallization as reported in the literature VARIOUS techniques have been used to identify the recovery, recrystallization, and grain growth processes that occur when cold-worked metals are annealed. As early as 1928 work was conducted that indicated measurable density changes occur when cold-worked single crystals of brass are annealed.' More recently, work by Murphy exhibited a corre- lation of density with microstructural changes observed on annealing cold-worked polycrystalline a brass.2 Other investigators have performed similar work on a brass and copper.324 In reviewing the literature, it was apparent that density work had been limited to fcc materials. Therefore, it was the purpose of this investigation to determine the density changes that accompany annealing the cold-worked bcc material, molybdenum. Two degrees of cold work, 30 and 90 pct reduction of cross-sectional area by rolling, were selected for this study. EXPERIMENTAL PROCEDURE High-purity vacuum arc-cast molybdenum was used in this study, the principal impurity being carbon in the amount of 80 ppm. The final rolling reductions were made at 1200°C in grooved rolls to provide 5/8-in.-diam rod. Density specimens 0.500 in. diam by 1.5 in. long were machined from the bar stock. The specimens were ground to the final dimensions to provide a smooth surface. Density measurements were made using a hydrostatic technique similar to that used by ~urphy.' This type of equipment permitted weighing in liquid immediately after the air weighing. During each weighing the temperature of the air and liquid was controlled to within 0.0l°C. This was accomplished by sealing the analytical balance in an air-tight brass chamber and surrounding it by an insulated wooden case. Preheated air was circulated in the air space between the brass chamber and wooden case by means of a blower. The temperature of the

Jan 1, 1964

By B. Amero, W. Petruk, D. R. Owens, D. R. Morris

Samples taken at different heights in the lead blast furnace of Brunswick Mining and Smelting corporation were studied to determine the phases present in order to interpret the reactions In the furnace. The main phases in the blast furnace feed are Pb3Ca2S13011, Zn ferrite (ZnFe204), and hardystonite (Ca2ZnSi207); rninor ones include lead and a Pb silicate. The temperature in the furnace varies from about 300°C at 4.2 m above the tuyeres to 1150°C at 1.1 m. There is no evidence of reactions in samples from points cooler than 800°C. Some reaction occurs between 950° and llOO°C and the lead sinter is nearly decomposed at about 1150°C. The first evidence of reaction was the decomposition of Pb silicate to lead and S102. At higher temperatures the Pb Ca2Si3011 decomposed to form lead and hardystonite (Ca2ZnS120rf. The Zn required for hardystonite was derived from the Zn ferrite which apparently re-equilibrated to a new Zn ferrite with less Zn. The decomposed sinter consists essentially of lead, hardystonite, wustite and a Zn ferrite with a low Zn content.

Jan 1, 1984

By Heinrich Siemes, Christa Hennig-Michaeli

The effect of temperature and orientation on the plastic behaviour of an impure titaniferous magnetite from Palabora (South Africa) has been investigated. Prismatic specimens were axially compressed along [001], [110] and [111]. The strain rate was about 3.10-6 s-1. Trace analyses of glide lines revealed a plastic anisotropy due to glide on several non-equivalent crystallographic planes. At 200 °C {111}<112> twinning, {111}<110> slip and {100}<011> slip have been operative. At 400 °C {111}<110> slip and {100}<011> slip are primary glide modes. {110}<110> slip seems to be a secondary glide mode in the [001] specimens at 400 °C. {III}<112> twin glide generates isolated sharp lamellae. {111}<110> slip produces smooth surface striae. {100}<011> slip is characterized by coarse and partially wavy slip bands. {I10}<110> slip displays faint remarkably equidistant glide lines. The critical resolved shear stresses (CRSS) decrease with rise of temperature. The CRSS ratio of slip on [100) to slip on {lll} increases from 1.1 at 200 °C to 1.4 at 400 °C giving rise to a distinct flow anisotropy of the magnetite at 400 °C.

Jan 1, 1982

By HAROLD VINTON COES

MANAGEMENT has been tersely defined as getting things done through the efforts of other people; but before we proceed further, let us distinguish between administration, management, and organization. Oliver Sheldon in his book, "The Philosophy of Management," offers the following definitions: Administration is the function in industry concerned in the determination of the corporate policy, the co-ordination of finance, production, and distribution, the settlement of the compass of the organization, and the ultimate control of the executive.

Jan 1, 1943

By J. J. Friel, E. S. Erickson

Dolomite-fluxed pellets of various compositions were made from magnetite concentrate, hematite concentrate and a concentrate containing a natural mixture of both. Physical properties and reduction test results were used to ascertain proper compositions and firing temperatures. These pellets were subjected to physical tests and to reduction tests. Petrographic and electron microprobe examinations were made to evaluate the effect of composition and fining on the phase assemblage. We interpreted our test results in terms of chemistry and microstructure and related these to properties. This approach enabled w to determine the composition best suited to each of the three concentrates. Compared with acid pellets, dolomite- fluxed pellets of the optimum compositions had similar physical properties but swelled less, softened at a higher temperature, and reduced faster and more completely.

Jan 1, 1983

By G. D. Cody, D. S. Beers, B. Abeles

The thermal diffusivity (thermal conductivity divided by specific heat) of Armco iron has been measured over the temperature range 30º to 1025ºC. The results are in good agreement with the thermal diffusivity computed from published values of thermal conductivity and specific heat, except near the Curie point and at the a to y phase transition, where the measured diffusivity undergoes rabid variations. The differences observed are ascribed to a rapid variation in the electronic thermal conductivity near the Curie point, and a decrease in the lattice thermal conductivity, at the a to ? phase transition. A major difficulty in measuring the thermal conductivity of materials at high temperatures is the determination and elimination of radiation losses. It has been shown, however, that in measuring thermal diffusivity D (thermal conductivity/specific heat) radiation losses can be taken into account exactly.&apos; In order to test the performance of a newly designed apparatus for measuring thermal diffusivity of solids,&apos; we measured Armco iron to an accuracy of 2 pct in the temperature range 30" to 1025°C. This material was selected since both the thermal conductivity,3&apos;4 k, and specific heat,5 C, are known accurately in this temperature range and thus the measured values of D could be compared with D computed from the pub-

Jan 1, 1962

By Gordon S. Duncan

The U. S. Geological Survey, I believe, has almost completed a study of the Harney Peak quadrangle, preliminary to the publication of a report on that district. As I was engaged for some months on an investigation of the mode of occurrence of the ore-bearing formation in this area, it has seemed to me timely to make public the results of my study, as a contribution to the consideration of this subject. It seems scarcely necessary to describe the locality and general geology of the Black hills of South Dakota, for since 1846 many have contributed information concerning this region, some of the reports bearing such well-known names as those of Walter P. Jenney, Henry Newton, S. F. Emmons, and C. R. Van Hise, while me have only to glance at Bulletin No. 4 of the South Dakota School of Mines, in which Prof. C. C. O&apos;Harra, of that institution, has given us a bibliography of contributions to the geography and geology of the section, to find that other well-known men have studied the district, and have given us the benefit of their researches. The U. S. Geological Survey has made geological maps of nearly the whole of the Black hills, the only quadrangle yet to be conlpleted being, as stated, the Harney Peak district. During the late summer and autumn of 1910, it was my lot to examine and report on a considerable area in this neighborhood, which once had been prospected, and in some cases exploited, for tin. This paper gives an account of certain geological phenomena, noted at that time, which greatly influenced my conclusions. The predominating formation of the district is pre-Cambrian, represented by a highly-cleaved mica-schist, usually very gar-netiferous, and sometimes hornblendic. Rising like an island from the surrounding schist is a large mass of granite, known as

Jan 1, 1913

By Homer N. Mead

This report develops equations for decline curve analysis based upon the premise that the rate of change of the reciprocal of decline for succeeding time intervals is constant when the reservoir is produced under a fixed set of conditions. A method is shown for predicting maximum production rate against cumulative production for any reservoir. A method is also presented for predicting future production rate by an analysis of past production performance after decline has been esrahlished. INTRODUCTION No significant contribution to the analysis of decline curves by the loss-ratio method has been made since J. J. Arps paper1. The concept of loss-ratio that was developed by Arps and his contemporaries has been redefined in another way and the concept of instantaneous loss-ratio at time zero has been added. In the mathematical developmerit by Arps, production rate was related as a continuous function with time and his equatlons were developed on that basis. In this paper, production is considered to be a series of segments for equal time intervals and equations have been developed based upon these finite differences. It is realized that decline curve analysis is not the answer to all predictions of reservoir behavior. However, as production must decline from an initial maximum rate to zero in any reservoir, if such decline can be expressed as an infinite series, this series should accurately predict production. Decline curve analysis should be considered a valuable tool that may be used in conjunction with predictions of future recoveries by other methods. Various uses of the decline curve method will be discussed in this paper. Equations predicting production rate at any time and cumulative production by exponential and hyperbolic decline will be developed. Characteristic values of b related to various types of drive will be discussed. After that a hypothetical reservoir will be studied and ultimate recovery by natural depletion and pressure maintenance compared, then actual field examples will be shown and discussed. The rate-cumulative curve introduced by H. N. Marshs in 1928 is an important one for use in estimating future production rate and ultimate recovery. This graphical method is the one that is used in conjunction with the equations to be developed for predicting production behavior. EXPONENTIAL DECLINE In exponential decline each succeeding production rate per unit of time is a constant percentage of the production rate just before it. Since (1 — r) is the common ratio, where r is the constant decline rate, this condition may be expressed as a geometrical progression; thus Pn = P (1 - r)n-1 . ......(1) Where r is less than unity, r Since P1 (1 - r)n = Pn+1 P1 - Pn+1 C =P1-Pn+1/r........(2) LOSS-RATIO In this paper the calculation for loss-ratio has been changed from the method presented by Johnson and Bollens2. The first loss-ratio to be calculated is a,; it is the initial production per unit of time after decline has set in divided by the difference between the initial and the second production rate. This loss-ratio is for the first time interval. After b (which is the constant change

Jan 1, 1957

By John W. Bell

The aim of the laboratory experiments described in this paper was twofold: 1. To measure as accurately as possible the maximum amount of crushing that can be effected by 1 hp. acting for 24 hr., by the two proposed methods for measuring the amount of crushing, namely: (a) by Rittinger&apos;s method; (b) by Stadler&apos;s method, based on Kick&apos;s law. 2. To show, if possible, that by one of these methods, the amount of crushing produced by 1 hp. in 24 hr. is a constant amount throughout a wide range in the diameter of the piece crushed, and that by the other method, the amount of crushing is a variable quantity over the same range of diameter; or else show that neither of the proposed methods for measuring the amount of crushing indicates a fixed relation between power and crushing and consequently a new method for computing this amount will have to be found to permit the establishment of a law of crushing. Experimental Methods Testing machines, calorimetric methods and commercial types of rock-crushing machines were considered with reference to their value for measuring power used in crushing. The following electrically driven crushing machines, installed and available in the McGill Ore-dressing Laboratory and which had been used in previous rock-crushing tests, on the whole seemed especially suited to the investigation: (1) Comet "A" crusher; (2) 7 by 9-in. Dodge crusher; (3) 10 by 16-in. rolls. In later tests a 3 ½-ft. Huntington mill was used.

Jan 1, 1918

By Freeman Bishop

Mercury is the latest ecological disaster. It was believed to be no pollution problem because it is heavier than water and expected to fall to the bottom of streams. But the Food and Drug Administration (FDA) found that mercury in a dozen states and several Canadian provinces was being ingested by fish. A Deadly Dose First to sound the alarm was Canada when a graduate student&apos;s research revealed that mercury contamination in Lake St. Clair had reached 1.4 pmm. which is almost three times the 0.5 ppm the FDA&apos;s allowable maximum.

Jan 1, 1970

H. H. Kellogg (Columbia University)—The accurate measurements of the equilibrium gas ratios for the reaction: Pb(1) + H2S = PbS(c) + H2 [I] reported in this paper are a distinct contribution to the literature, and the authors are to be congratulated. I wish to comment, however, on the correlation of the data which is presented. The authors show a straight line correlation of log H2S/H2 vs 1/T, Fig. 1, and are satisfied with this for calculation of ?Fo even when extrapolated to low temperature (427 °C). Heat capacity data for the constituents of this reaction are available (at least to 900°K), however, and ACP for reaction [I] is finite and positive in the temperature range studied. Simplification of the heat capacity equations yields: ?CP= 2.71 + 1.65 x 10-3T (298°-900°K) This positive value of ?CP should result in a small but noticeable curvature of a plot of log K vs 1/T. That the experimental data fail to show such a curvature may be traced to another oversimplification of the author&apos;s treatment of their data. They assume that the activity of liquid lead is unity for all temperatures, so that

Jan 1, 1961

JAMES GAYLEY (President), R W RAYMOND (Secretary), FRANK LYMAN Treasurer) T A RICKARD NEW YORK, N Y CHARLES H SNOW NEW YORK, N Y R W RAYMOND NEW YORK, N Y (Terms expire February, 1906 ) JAMES GAYLEY NEW YORK, N Y FRANK KLEPETKO NEW YORK, N Y FRANK LYMAN NEW YORK, N Y (Terms expire February, 1907 ) JAMES DOUGLAS NEW YORK, N Y JAMES F KEMP NEW YORK, N Y ALBERT R LEDOUX NEW YORK, N Y (Terms expire February, 1908 ) Council PRESIDENT OF THE COUNCIL JAMES GAYLEY VICE-PRESIDENTS OF THE COUNCIL GEORGE W MAYNARD NEW YORK, N Y JULIAN KENNEDY PITTSBURG, PA CHARLES D WALCOTT WASHINGTON, D C (Terms expire February, 1906 ) WILLIAM P BLAKE TUCSON, ARIZ THOMAS F COLE ,DULUIH, MIFF IRVING A STEARNS WILKES-BARRE, PA (terms expire February, 1907 )

Jan 1, 1910

ALASKA Established November 19, 1947 Regular meetings fourth Monday of each month except June, July, and August Theodore A Loftus, Chairman John C Boswell, Vice-Chairman Patrick H O&apos;Neill, Secretary-Treasurer Box 1034, Fairbanks, Alaska District Vice-Chairmen Robert L Thorne, Juneau, Alaska Alfred J Lomen, Jr , Nome, Alaska Donald G. Wilcox, Anchorage, Alaska

Jan 1, 1952

By John Bell

Aim of Rock-Crushing Experiments THE aim of the laboratory experiments described in this paper was twofold: 1. To measure as accurately, as possible the maximum amount of crushing that can be effected by 1 hp. acting for 24 hr., by the two proposed methods for measuring the amount of crushing, namely: (a) by Rittinger&apos;s method; (b) by Stadler&apos;s method, based on Kick&apos;s law. 2. To show, if possible, that by one of these methods, the amount of crushing produced by 1 hp. in 24 hr. is a constant amount throughout a wide range in the diameter of the piece crushed, and that by the other method, the amount of crushing is a variable quantity over the same range of diameter; or else show that neither of the proposed methods for measuring the amount of crushing indicates a fixed relation between power and crushing and consequently a new method for computing this amount will have to be found to permit the establishment of a law of crushing. Experimental Methods Testing machines, calorimetric methods and commercial. types of rock-crushing machines were considered with reference to their value for measuring power used in crushing. The following electrically driven crushing machines, installed and available in the McGill Ore-dressing Laboratory and which had been used in previous rock-crushing tests, on the whole seemed especially suited to the investigation: (1) Comet "A" crusher; (2) 7 by 9-in. Dodge crusher; (3) 10 by 16-in. rolls. In later tests a 3 ½ -ft. Huntington mill was used.

Jan 2, 1917

By E. I. Alessandrini, A. U. Seybolt

Selective oxidation (preferential oxidation of a single alloy component) can be an important oxidation mode in the case of alloys such as Si-Fe, Al-Fe, and so on, when heat-treating in atmospheres of low oxygen potential. It was the purpose of this work to identify the oxide films formed on iron containing 31/4 pct Si at low oxygen potentials, and to make some observations on the H2O/H2 ratios required to form them. EXPERIMENTAL METHOD HYDROGEN of varying water content offers a very convenient method of establishing a wide range of oxidizing power, or oxygen potential. The method chosen to provide a desired H2O/H2 ratio was to nearly saturate hydrogen at room temperature by bubbling the gas through water at room temperature, and then to wring out the excess water by passing the wet gas through a long glass spiral immersed in a refrigerated liquid at a desired dew point. After oxidation, the samples were examined by electron diffraction in order to identify any film which might be present. PREPARATION AND TREATMENT OF SAMPLES The samples were prepared from a Si-Fe alloy made in the laboratory using electrolytic iron and 96 pct ferro-silico11, vacuum-induction melted, hot-rolled then cold-rolled to 0.015-in. thickness. After the cold-rolling the samples were annealed at 1000°C. Transmission Laue X-ray patterns showed very little evidence of preferred orientation, but it is likely that a weak texture could have escaped notice. The chemical analysis was as follows: 3.34 Si, 0.01 Al, 0.001 0, 0.006 C, 0.002 N. Before each sample was oxidized, it was polished through 4/0 emery paper, cleaned and dried using benzene, carbon tetrachloride, acetone, absolute alcohol, and ether. The method of oxidizing the samples was as follows: Samples about 1/2 by 1 by 0.015 in. were held in the upper, cool part of a vertical vacuum furnace until the desired temperature was established in the furnace, Fig. 1. The sample was then lowered into the uniform hot zone where it was heated quickly to the desired temperature, and subjected to hydrogen of controlled moisture content (dew point) as mentioned previously. Temperatures from 400" to 1000°C were used, and dew points from room temperature to —78°C were explored. In general, the runs lasted about 6 hr, but a few runs were of different duration, as will be indicated later. After the predetermined period of time had elapsed, the specimens were withdrawn by the hollow stainless steel-quartz holder to a cool zone at the top of the furnace. EXPERIMENTAL RESULTS The results are summarized in Table I. Most of the electron-diffraction patterns were obtained by glancing-angle reflection, but in a few cases it was possible to strip the oxide films from the surface by a total immersion in a 3 pct bromine-methanol solution. Some of the thinner stripped films yielded quite satisfactory transmission patterns. However, both diffraction techniques yielded the same results; the patterns while most frequently showing a (low) tridymite, also showed a (low) cristobalite in some cases. A few patterns showed evidence of both phases. Because of the known nonequilibrium behavior of silica, it is not surprising that both forms of silica could coexist on one sample. It was noted that at fairly low dew points such as —40°C, there was a tendency for diffuse diffraction rings, suggesting a very small crystallite size. Also some subsequent experiments to be reported later show that thin silica films can be amorphous.

Jan 1, 1959

By A. E. Jenkins, A. Jostsons

Isothermal sections of the Ti-0-H phase diagvam at 600°, 700°, and 800°C have been constructed from equilibrium hydrogen pressure measurements over a range of Ti-0-H alloys containing up to 34 at. pct 0. Oxygen reduces the hydrogen solubility at fixed hydrogen pressure but increases the terminal solubility in the a solid solutions at the a/(a + P) phase boundary. Metal-lographic studies of alloys annealed below the eutectoid temperature show that oxygen also increases the ter-ninal solubility of hydrogen in the a solid solution in equilibrium with the hydride phase. The effect of oxygen on hydrogen solubility is discussed in terms of the electronic and geometric structure of interstitial solid solutions. THE isothermal solubility of hydrogen in a Ti-0 alloys at 800°C has been measured by Hepworth and ~chuhmann&apos; who subsequently used ternary Gibbs-Duhem integrations to calculate oxygen activities in binary Ti-0 alloys. The present study aims to extend Hepworth and Schuhmann&apos;s measurements to alloys richer in oxygen and to a range of temperatures. This paper presents the results of hydrogen equilibrium pressure/concentration measurements in Ti-0 alloys as well as observations on the effect of oxygen on the terminal solubility of hydrogen in a titanium. The thermodynamic properties of binary Ti-0 alloys, derived from these measurements, will be published separately.&apos; EXPERIMENTAL METHODS Specimen Preparation. Ti-0 alloys were prepared from iodide-refined titanium and titanium dioxide obtained by hydrolysis of redistilled titanium tetrachlo- ride. Specimens containing up to 16 at. pct 0 were prepared by electromagnetic levitation3 whereas a conventional tungsten arc furnace with a water-cooled copper hearth was used to melt oxygen-rich alloys. The specimen homogeneity was indicated by the constancy of lattice parameters of samples from various parts of the ingot as well as by the sharpness of the reflections on X-ray powder patterns. Oxygen-rich specimens in the composition range (20 to 34 at. pct), where ordering has been ~bserved,~ were annealed for 300 hr at 600°C prior to use in hydrogen solubility measurements. Apparatus. The hydrogen pressure/concentration measurements were made with a modified Sieverts apparatus shown diagrammatically in Fig. 1. Specimens were placed in a clear silica tube and impurity pickup by direct reaction with silica was prevented by lining the heated end of the silica tube with thin molybdenum sheet. A double silica tube was required to eliminate loss of hydrogen by diffusion through silica at high temperatures and high hydrogen pressures, the space between the tubes being maintained at a hydrogen pressure equal to that above the specimen. Hydrogen was purified by diffusion through a Ag-Pd tube.= Hydrogen pressures were measured with a mercury McLeod gage in the range 0.001 to 4 Torr

Jan 1, 1968