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By S. R. Goodman, Hsun Hu

A detailed study of texture developmenf in poly crystalline copper atzd 70-30 brass has been completed. Textural changes as a function of deformation are shoum by pole jigmres and by intensity measurements oF- various rejlectiotzs from the rolling plane and the rolling direction. These examinations were accompanied by measurements of stacking fault frequency, hardness changes, and microstructure. Some of the results were briefly presented earlier. Additional results reported here are consistent with the idea that deformation faulting or slip by partial dislocations is of primary importance in the formation of deformation textures in fcc metals. lo examine the idea that deformation faulting is of primary importance in determining whether the texture is the copper type or the brass type an extensive study of the development of polycrystalline textures in copper and 70-30 brass was initiated. Besides the determination of complete pole figures, the intensities of the various reflections from both the rolling plane and the plane perpendicular to the rolling direction, the peak shifts due to deformation stacking faults, and the hardness of the rolled specimens were examined at various reductions from 10 to 99 or 99.5 pct. Mi-crostructures were examined by transmission electron microscopy. Some of the results were briefly presented in an earlier publication.' Since then, additional information has been obtained. This is given in the present paper. EXPERIMENTAL PROCEDURE Material and Specimen Preparation. The material used was a commercial electrolytic copper bar 1i in. wide and 2 in. thick and a 70-30 brass bar la in. wide and 1i in. thick. Chemical analysis indicated a purity of 99.97 pct for the copper, with 0.025 pct 0 as the major impurity. The 70-30 brass was of higher purity with 0.0016 pct 0 as the major impurity. Extreme care was taken in the preparation of the starting material to insure uniformly fine grains with a nearly random initial texture. The two bars were first cold-forged and then annealed to eliminate any original texture. The grains were then refined by several cold rolling (approx 30 pct reduction) and annealing treatments. The + -hr anneals were carried out in a salt bath at 390" to 440°C for copper and at 490°C for brass. The resulting penultimate grain size was 0.06 mm for copper and 0.03 mm for brass, and both showed very little preferred orientation. The number of prior cold rolling and annealing cycles was such that the final thickness after various final reductions of 10 to 95 (for brass) or 99 (for copper) pct was the same (0.020 in.). These annealed strips were rolled in two directions by reversing end for end between passes according to the following schedule: 0.006 in. per pass to 0.100 in., 0.003 in. per pass to 0.050 in., 0.002 in. per pass to 0.025 in., 0.001 in. per pass to 0.020 in. Texture Determination. The development of rolling textures was studied by examining complete pole figures determined from the (111) reflection. Specimens thinned from one face of the strip to half thickness (0.010 in.) were used to obtain the central portion of the pole figures, while specimens thinned from both faces to 0.003 in. were used to obtain the peripheral portion. The reflection and transmission techniques have been described previously. In addition to X-rav pole figures, texture development was also studied b; examining the intensity variation of the (Ill), (200), (2201, (311), (331), (420), and (442) reflections from the rolling plane and from the plane normal to the rolling direction, as a function of deformation. The same specimens used for the central portion of the pole figures were used for the intensity measurements of the various reflections from the rolling plane. For intensity measurements from the plane normal to the rolling direction, composite specimens were prepared by mounting sections cut parallel to the transverse direction of the strip. An epoxy resin was used to bond these sections together, and the entire composite was then mounted in a cold-setting resin to facilitate subsequent polishing and etching to remove distorted metal at the cut. The intensities were expressed in units of the integrated intensities measured from an annealed copper specimen having almost no preferred orientation. Stacking Fault Frequency Determination. Following the analysis of Warren: the stacking fault frequency, a, was determined from the change in the peak separation (A%) of two neighboring reflections of a deformed specimen, as compared with the normal peak separations of a fully annealed specimen. To obtain sufficient intensities for the second-order reflections, (222) and (400), composite specimens were prepared from parallel sections cut from the strip at 30 deg to the rolling direction for copper and 25 deg for the brass.* From texture data, these sections are known to contain a large population of both (111) and (200) planes. Since residual stresses can also cause X-ray line shifts (the direction of line shifts depends upon the sign of the stress), the use of composite specimens consisting of sectioned planes should help compensate for these effects as the residual stresses change sign from the surface to the central section of a rolled strip. Since the amount of peak shift is almost un-measurable in brass rolled 15 pct and in copper rolled

Jan 1, 1969

By C. Ernest Birchenall, Gerd M. Rosenblatt

The pressure and molecular weight of the antimony vapor over solid solutions of tin in antimony, containing 97.4, 94.9, 93.0, and 90.7 at. pct Sb, have been measured from 445° to 545°C by the torsion-effision method. The vapor is all Sb, within experimental error. A solidus curve which differs somewhat from the accepted curve has been calculated using the measured antimony activities. Metallographic examination of additional annealed alloys substantiates the accepted solidus. The solid solutions, which show negative deviations from ideality, probably do not deviate greatly from regular solution behavior. HANSEN' considers the Sb-Sn phase diagram to be well established with the exception of the boundary of the (Sb) phase.* Although there have been no pre- Their data can be combined with data for the solid alloys to calculate the solidus curve of the (Sb) phase. This paper presents measurements of the pressure ant1 molecular weight of antimony over Sb-Sn solid solutions containing 97.4, 94.9, 93.0, and 90.7 at. pct sb. Measurements were made by simultaneous use of the volmer3 torsion and Knudsen, effusion methods. The results of these measurements have been combined with the vapor pressure of pure antimony5 to obtain the activity of antimony in the primary solid solutions. The solidus curve calculated from these data differs somewhat from the accepted curve and is rather uncertain. Metallographic examination of Sb-Sn alloys was carried out to clarify the position of the solidus of the (Sb) phase. EXPERIMENTAL The apparatus and technique have been described previously.5 The measurements were made with the same effusion cells and torsion wire used in the measurements on pure antimony. The torsion measurements were calibrated with mercury at 30" using a mercury vapor pressure of 2.96 x 10-3 mm Hg determined by concurrent, absolute, weight-loss experiments. As in the measurements on pure antimony, an extraneous vapor was observed to distill off during the first run after the cell had been loaded with A fresh sample of alloy and during the first minute or two of every run. The change in composition after a series of runs with one sample was of the order of 0.1 at. pct and thus completely negligible in the calculation of the thermodynamic properties. The alloys were prepared from pieces of Merck antimony and Matheson, Coleman, and Bell reagent-

Jan 1, 1962

US 4,134,944-Production of iron oxide ore pellets of uniform size and excellent strength. Small pieces of ore are rolled into nuclei in a first pellet-rolling circuit in the presence of a binder, the nuclei sized and hardened by sintering or cold-bonding of the binder, the nuclei rolled in additional ore to form product pellets, the pellets sized, the suitable size fraction taken as product, and undersize pellets returned to the rolling operation. P. A. Ilmoni and R. Drugge, assigned to Luossavaara-Kiirunavaara AB Jan 16, 1979. 5 pp. (264-37) Filed- 5-25-77 (800,278) Priority: Sweden, 6-2-76 (76/06,¬241). Same British 1,553,763, dated Oct 10, 1979. US 4,145,210-In the induration of pellets of iron oxide ore or iron works dust or sludge, a charge of dried pellets and 2-20% by weight of coke having a size range of from 5 to 30 mm, a drum index of more than 70, a reactivity index of less than 50, and a tumbler index of more than 50 is charged into a rotary kiln The charge is heated and passed through the rotating kiln to indurate the dried pellets without burning the coke Powder-coated coke is recovered from the kiln for reuse. Ring formation in the kiln is substantially prevented. K. Kato and K Kadota, assigned to Sumitomo Metal Industries, Ltd, and Sumitomo Heavy Industries, Ltd. Mar 20, 1979 10 pp (75-3) Filed- 2-22-77 (770,947) Priority: Japan, 2-24-76 (51/19,754) US 4,145,211-Method of cooling hot metallized iron oxide ore agglomerates from a direct reduction furnace Agglomer¬ates ranging from 3/a in to 41/2 in in cross-section and at a temperature of 1000-2000°F are formed into a moving bed while at rest relative to each other Air at ambient tempera¬ture is passed through the bed at a velocity sufficient to cool the agglomerates rapidly to a temperature no greater than about 500°F without substantial reoxidation of the metal in the agglomerates and by using air as the sole cooling gas. C A Czako, A Berzins, and M J Greaves, assigned to Arthur G McKee & Co Mar. 20, 1979 15 pp. (75-34) Filed: 7-18-77 (816,467)

Jan 1, 1980

By Henry S. Burnholz, Charles Y. Clayton, Francis B. Foley

This work was first undertaken for the U. S. Bureau of Mines, in 1919-20, by C. E. Julihn, superintendent of the station at Minneapolis. Learning of the interest, in this subject, of B. F. Tillson, of the New Jersey Zinc Co., Mr. Julihn and Mr. Foley went to Franklin, N. J., and discussed the matter with him. A conference in Chicago, in November, 1920, was attended by Dr. F. G. Cottrell, who was then Director of the Bureau of Mines, and representatives of the Bureau of Mines and of the hlissouri School of Mines and Metallurgy; at this time a cooperative plan of work was agreed upon by the Bureau of Mines and the Missouri School of Mines. In February, 1921, Mr. 'Tillson arranged a conference on this subject at the time of the annual meeting of the American Institute of Mining and Metallurgical Engineers, at which several technical papers were presented. In a paper, the Breakage and Heat Treatment of Hock Drill Stcels, he suggested a program that might be carried out in connection with the investigation of the problem. At this conference Mr. Manning, former Director of the Bureau of Mines, suggested the formation of an advisory committee to the Bureaus of Mines and of Standards for prosecution of this investigation. On Feb. 20, 1922, a secoud conference in New York, at the time of the annual meeting of the American Institute of mlining and Metallurgical Engineers, was attended by representatives of various technical societies. At this meeting, the report of Nov. 20, 1921, of the Chiefs of Divisions of Metallurgy of the Bureaus of Mines and of Standards, was discussed and it was agreed: 1. That the survey recommended by the two bureaus should be undertaken, which survey would have for its object the ascertaining of the present status of the practice of the heat treatment of drill steels, the extent to which the breakage occurs, etc.; and 2. That a report should be presented, of the findings of those who made the survey, to the Advisory Board to the Bureaus of Mines and of Standards. The Bureau of Standards assigned $4000 to the prosecution 01 a three-months' survey, which was carried out in April, May, and June, 1922, of about sixty mines

Jan 1, 1923

By Charles Y. Clayton, Henry S. Burnholz, Francis B. Foley

This work was first undertaken for the U. S. Bureau of Mines, in 1919-20, by C. E. Julihn, superintendent of the station at Minneapolis. Learning of the interest, in this subject, of B. F. Tillson, of the New Jersey Zinc Co., Mr. Julihn and Mr. Foley went to Franklin, N. J., and discussed the matter with him. A conference in Chicago, in November, 1920, was attended by Dr. F. G. Cottrell, who was then Director of the Bureau of Mines, and representatives of the Bureau of Mines and of the hlissouri School of Mines and Metallurgy; at this time a cooperative plan of work was agreed upon by the Bureau of Mines and the Missouri School of Mines. In February, 1921, Mr. 'Tillson arranged a conference on this subject at the time of the annual meeting of the American Institute of Mining and Metallurgical Engineers, at which several technical papers were presented. In a paper, the Breakage and Heat Treatment of Hock Drill Stcels, he suggested a program that might be carried out in connection with the investigation of the problem. At this conference Mr. Manning, former Director of the Bureau of Mines, suggested the formation of an advisory committee to the Bureaus of Mines and of Standards for prosecution of this investigation. On Feb. 20, 1922, a secoud conference in New York, at the time of the annual meeting of the American Institute of mlining and Metallurgical Engineers, was attended by representatives of various technical societies. At this meeting, the report of Nov. 20, 1921, of the Chiefs of Divisions of Metallurgy of the Bureaus of Mines and of Standards, was discussed and it was agreed: 1. That the survey recommended by the two bureaus should be undertaken, which survey would have for its object the ascertaining of the present status of the practice of the heat treatment of drill steels, the extent to which the breakage occurs, etc.; and 2. That a report should be presented, of the findings of those who made the survey, to the Advisory Board to the Bureaus of Mines and of Standards. The Bureau of Standards assigned $4000 to the prosecution 01 a three-months' survey, which was carried out in April, May, and June, 1922, of about sixty mines

Jan 1, 1923

By Stirling Huntley, R. H. Johnson

Pennsylvania will be remembered, as long as oil is produced, as the cradle of the industry of petroleum in North America. It was on Oil Creek, near Titusville, Venango Co., that Col. Edwin L. Drake, superintendent for the Seneca Oil Co., brought in the first commercial oil well on Aug. 28, 1859. Great difficulty was experienced in getting the well down to the producing depth of 69 ft. (21 m.) with the spring-pole system then in vogue for punching shallow water wells, so the novel expedient of driving an iron tube through the surface clays and quicksand was finally resorted to. The well had an initial yield of 25 bbl. a day on the pump, but soon went off, though 2000 bbl. were produced by the end of the year. With the Drake well a success, a young industry sprang into being, the rapid growth of which has been second to none in the country and the value of whose product is only surpassed by that of coal. For years the only producing territory, the Pennsylvania-New York field attained its greatest production in 1891, when the bringing in of the McDonald pool, between Pittsburgh and the West Virginia line, gave a total of over 33,000,000 bbl. At present the field, combined with West Virginia and southeast Ohio, gives 25,000,000 barrels. Geology and Stratigraphy In general, the Appalachian field is a huge geosyncline, the axis of which runs roughly northeast-seuthwest, from north of the New York state line south through Brookeville, Kittanning, Pittsburgh, Washington, through the southwest corner of the state of Pennsylvania into West Virginia. Minor folding has accompanied or followed the dominant fold of the field, and it is from these structures near the Pennsylvania-West Virginia line and their influence on the accumulation of oil and gas that I. C. White, state geologist of West Virginia, obtained his evidence for anticlinal guidance of prospecting. Many horizons in the geologic column of the field serve as reservoirs, and there arc several pools that have wells producing side by side from different and widely vertically separated strata. The strata show a promising succession of porous sand and conglomerate horizons alternating with numerous gray and dark brown 01. black shales, admittedly

Jan 1, 1921

AN intermetallic compound, Ni3A1, has an ordered fcc structure of type Ll2, and shows peculiar dependence of the yield stress upon temperature; i.e., the yield stress increases by a factor of six upon raising the temperature from 77" to 900K1, 2 This compound is technologically important, since many nickel-base superalloys owe their high-temperature strength to the peculiar yield stress behavior of Ni3Al. The only study of the elastic behavior of this compound was made by Davies and Stoloff,1 who determined Young's modulus of poly crystalline Ni3A1 between 300" and 730°K. The determination of single-crystal elastic constants of Ni3A1 is therefore of interest in connection with dislocation dynamics and is reported in this paper. A single-crystal specimen, 1 by 1 by 3 cm, was cut from an ingot generously supplied by Dr. B. H. Kear of Pratt & Whitney Aircraft. Following initial machining with a Servomet and a surface grinder, the specimen was etched and annealed at 1100°C for 5 hr in vacuum followed by furnace cooling. Two parallel faces were oriented normal to within ±l deg of a [I101 crystallographic axis by the back-reflection Laue technique. The parallel faces were hand-lapped, etched, and polished by the usual metallographic procedures. Final thickness along the [I101 axis was (0.9325 * 0.0005) cm. Chemical analysis gave an average composition of 87.35 pct Ni. Total impurity content is esimated to be no more than 0.1 pct. The elastic constants were calculated from measurements of ultrasonic waves which were propagated along the [110] axis. A longitudinal wave and two shear waves whose displacements are aligned along the [ 110], [li~], and [001] directions, respectively, are necessary in order to completely specify the three elastic constants. Two 3/6-in. quartz transducers were bonded to the parallel faces of the sample with ~ac-seal.3 Although this bond was sensitive to thermal shock, it performed satisfactorily over the entire temperature range for both longitudinal and shear wave propagation. A frequency of 5 mHz was employed in the method of Williams and Lamb4 in order to measure the absolute value of the ultrasonic velocity. The pulse-overlap technique of Mcskimin5 was also used at this frequency in order to determine the shift in the ultrasonic velocity

Jan 1, 1970

By Lawrence Addicks

Some three years ago the smelter connected with the Chrome, N. J., refinery of the United States Metals Refining Co. found itself embarrassed by constantly increasing piles of unsmelted blast-furnace flue dust. The charge was fine and 10 to 15 per cent. of it was blown over into the flue. Sulphur was at that time too scarce to make the sintering of the finer part of the charge attractive, and raw-ore smelting in a reverberatory with a partly oxidized charge was not to be thought of. A great many schemes were considered, including leaching, blowing into the converters, and briquetting, the problem finally narrowing down to blast roasting and nodulizing. It was found by experiment that blast roasting would not yield a satisfactory sinter without the addition of coke dust or sulphide fines to augment the fuel value of the flue dust, and on this account, together with the low first cost of a kiln, the latter was decided upon. A couple of tons of flue dust were tried out in the experimental kiln in the laboratory at Yorktown, Va., of J. H. Payne, who acted as consulting engineer in this connection. This kiln was approximately 2 ft. in diameter and 20 ft. long and was fired with fuel oil. A run of several hours yielded excellent nodules. The ki1n showed no tendency to build in and form "nose rings" and gave a fuel consumption of 50 gal, of oil per ton of flue dust. There was no indication of any stack loss. The roasting was strongly oxidizing. A study of what full-size kilns were doing on cement clinker and on nodulizing pyrites cinder indicated that a 60 by 6 ft. kiln would certainly not consume over half of the oil per ton of flue dust shown on the test and as fuel oil at that time was selling around 2 1/2 c. per gallon it was decided to let it go at that. A 60 by 6 ft. kiln was decided on, as that size is standard in cement practice, although fast being replaced by much larger ones with their greater fuel economy, and as it fitted in the building space available. A 6-in. brick lining brought the net diameter down to 5 ft. The inclination

Jan 1, 1915

By A. D. Zunkel, A. H. Larson

Equilibrium arsenic contents of Pb-As alloys in contact with PbO-As2O3 slags containing less than 30 mol pct As2O3, were determined at 650°, 700: and 750 C in an inert at?rzosphere. In this temperature range, the arsenic content of the alloy increased with increasing temperature in the single-phase liquid slag region and decreased with increasing temperature in the two-phase slag region and the single-phase solid-solution slag region. The PbO-As2O3 phase diagram below 22 mol pct As2O3 was determined by thertrzal analysis and by application of a log ?As2O3/?PbO vS log XAs2o3 /x3pbO plot determined from the equilibrium actiuity data. The resulting phase diagram was not well-defined since the eutectic temperature was not detected in the thermal analysis experiments, although a region of terminal solid solubility of As2O3 was found. Results from the phase diagram determination are compared with an existing diagram in the literature. THIS experimental investigation is an extension of a study by the authors1 on the slag-metal equilibria in the systems concerned with commercial lead refining processes such as softening and dross fuming. The first part of this investigation was a study of the slag-metal equilibria in the Pb-PbO-Sb2O3 system. The only experimental work previously done on the Pb-PbO-As2O3 system was by Pelzel2,3 in which the phase diagram for the PbO-As2O3 system was determined below 50 wt pct As2O3 and the equilibrium constant for the reaction 3Pb + As2O3 + 3PbO + 2As was determined as a function of temperature. No slag-metal equilibrium data have been determined. It is due to the scarcity of information regarding the Pb-PbO-As203 system that this work was undertaken. This paper describes the determination of the slag-metal equilibria in the Pb-PbO-As203 system by equilibrating Pb-As alloys with PbO-As2O3 slags in an inert atmosphere, the effect of 1 wt pct additions of bismuth and copper on the slag-metal equilibria, and the PbO-As2O3 phase diagram both by thermal analysis and the use of the slag-metal equilibria data. EXPERIMENTAL Materials. The materials used in this investigation were analytical reagent-grade and assayed as follows: 1) 99.8 pct PbO (0.014 pct insoluble in CHJCOOH, 0.02 pct not precipitated by H2S, 0.1 pct CaO, and 0.08 pct SiO2); 2) 99.95 pct As2O3; 3) 99.99 pct Pb; 4) 99.0 pct As; 5) 99.99 pct Cu; and 6) 99.97 pct Bi. Room-temperature X-ray patterns revealed no detectable impurities in any of these materials. Apparatus for Equilibrium and Thermal-Analysis Determinations. The resistance-heated crucible furnace used in this investigation employed nichrome elements and was mounted so that it could be raised to surround the reaction tube during each experiment and, subsequently, lowered. A schematic diagram of the apparatus is shown in Fig. 1. Each charge was heated in a 3+-in.-OD by 31/2-in.-high 416 stainless-steel crucible placed in a 41/4-in.-1D by 18-in.-long fused-silica reaction tube which was closed at one end. On a shoulder around the crucible was placed a 3: -in.-OD by 12-in.-long open-end fused-silica condenser tube. The open end of the reaction tube was covered by a water-cooled brass cap with ports for 1) admitting an inert atmosphere to the system through a stopcock, 2) introducing a stainless-steel, motor-driven, paddle stirrer into the crucible, 3) evacuating the system with a mechanical vacuum pump, and 4) sampling the melt with Vycor sampling tubes. The brass cap was fitted to the open end of the reaction tube with a silicone gasket and collar clamp. The furnace temperature was controlled by a Barber-Coleman Capacitrol controller and a chromel-alumel thermocouple. Due to the corrosiveness of the melt, the controlling thermocouple also served as the measuring thermocouple. The temperature of the melt was calibrated against the controller temperature and was checked periodically during each test with a Vycor-enclosed calibrated chromel-alumel thermocouple. The temperature measurement and control can be considered accurate to ±3°C. Procedure. The charge placed in the crucible for each experiment consisted of 1000 g of Pb-As alloy and 300 g of PbO-As2O3 slag. The crucible was then placed in the reaction tube, the condenser tube was placed on the shoulder of the crucible, the silicone gasket and brass cap were fitted on the open end of the reaction tube, and the entire system was evacuated and filled with argon ten times. After the last flushing, a positive argon pressure of 1 psig was impressed on the system. The furnace was then raised to sur-

Jan 1, 1968

By C. E. Jackson, E. C. Nelson, A. L. Christenson

Much information regarding the transfornlatio~lal characteristics of a steel as it cools in a known manner from the austenitic state can be obtained from dilatometric studies. This method has received more arid more attention because of its great flexibility, accuracy, and ease of interpretation. 'The method is entirely applicable to any rate of heating and cooling although the experumental procrdures for high rates of cooling have offered some difficulties. This paper presents a description of equipment employing cooling rates up to 500 °C. per secorld and the results of dilatometric observations on six commercial steels are included. French and Klopsch1 studied the cooling transformations of a serirs OF carbon steel, using the thermal arrest method. This was followed by the systematic investigatiol1 of Esser and co-workers on the effect of carhon2 and other alloying additions. in which the transforlnation temperature\ were determined by magnetic induction measurements indicated by a string galranoineter. Emphasis was placed on determining Ar' trailsformations and the critical cooling rates for these steels. The maglietic measurements wrere used in an effort to obtain more accurate data at higher cooling rates. Measurements of thermal arrest were made also to check the validity of the magnetic indications, and good correlation was found between the two, although Esser's,Ar' temperature measurements on iron-carbon alloys were about 200°F. lower than the measurements made by Fresnch and Klopsch. A notable contril~ution by Esser was the introduction gas quenching. wever and Rose4 used a moving-coil galranometcr in the study of the .Ar and Ar" of iron-carbon alloys by the thermal arrest method and obtained somewhat lover Ar" temperatures than those observed by Esser below I per cent carbon and considerably higher ahove. They concluded that the cooling rate had little influcncc on the Ar" temperatures above 0.4 per cent carbon, although Esser had observed a decrease in the -4r" temperature with increasing cooling rate with similar steels. Digges determined the .Ar" temperature4 for a scries of high-purity iron-carbon alloys, and close agreement with his results was obtained by Greninger. The thermal arrest method. together with metallographic observation used in both these studies, represents the latest investigations of this type. Any investigation by thermal analyses is dependent on the heat of reaction and the specific heat of the

Jan 1, 1945

By P. T. Chiang

Chemical etching methods for the simultaneous revealing of the tellurium or selenium Phase and the chalcogenide grain boundaries of the alloy systems are given. A tellurium eutectic was found Present in zone-melted ingots. Similarly, a selenium monotectic was present in ingots. In general, the second phase (tellurium or seleniumn) occubies three different sites; viz., along the chalcogenide grain boundaries, as inclusions within the chalcogenide grain, and on the undersurface of the ingot. The detection limit for the tellurium phase is about 1 u in width. THERMOELECTRIC materials based on Group V (bismuth, antimony) and Group VI (selenium, tellurium) elements have aroused considerable interest in recent years in the practical application of thermoelectric cooling. In many cases, a small amount of excess tellurium (or selenium) was added to the material to optimize its thermoelectric properties. Then the question immediately arises as to the number of phases present in the resultant alloy. In the binary systems of Bi-Te, Sb-Te, and Bi-Se, the congruent melting compositions have been reported to be non-stoichiometric and are represented by Bi~Te respectively. It is to beexpected and known that Bi2Te3 and SbzTe3 crystallize from the melt with an excess of bismuth and antimony in the lattice and that tellurium forms a eutectic.~' The same could be assumed to take place in the pseudo binary systems of (Bi,Sb)zTe3 and Bi2(Se,Te)3 as well as in the system studiedby puotinen5 and other workers. Likewise, BiaSe3 crystallizes from the melt with an excess of bismuth in the lattice and selenium forms a monotectic.~ Therefore, in practice, alloys solidified from the melt often contain a second phase (tellurium or selenium) in one region or another of the solid mass even without the addition of excess tellurium (or selenium). ~u~~recht' studied the thermoelectric properties of (Bi,Sb)2Te3 alloys with excess tellurium and simultaneous additions of selenium. He mentioned that the materials show two phases because of the considerable excess of tellurium or selenium. However, he did not report as to how the tellurium or selenium phase was identified. It is generally believed that the presence of an excessive amount of tellurium or selenium phase in the alloy would adversely affect its thermoelectric properties and its uniformity. Consequently, there is a need for a simple method for the identification of the tellurium and selenium phase. The quantity of the second phase present is usually too small to be detected either by chemical analysis or by normal X-ray techniques. This investigation was therefore carried out, first, to devise a simple metallographic method for the identification of the tellurium or selenium phase coexisting with the chalcogenides and, second, to determine the distribution and specific location of the tellurium or selenium phase in the ingots. EXPERIMENTAL PROCEDURE The starting materials used for the alloy preparations were 99.999 pct pure bismuth, antimony, and tellurium and 99.997 pct pure selenium. The bismuth and antimony were obtained from Consolidated Mining and Smelting Co. of Canada Ltd., while the selenium and tellurium were obtained from Canadian Copper Refiners Ltd. The tellurium was purified further in the laboratory by zone refining. The elements were pulverized in a stainless-steel pestle and mortar. The amounts for the desired composition were weighed out each time on an analytical balance to make up a 100-g sample. Then the sample was introduced into a Vycor ampule (19 by 150 mm), pumped down to a vacuum of 10"5 Torr for 15 min, and sealed off. The ampule was then heated in a horizontal resistance furnace at 800" to 900°C for about 20 hr. During this period the assembly was rocked back and forth several times to ensure good mixing. At the end of the heating period, the ampule was quenched in cold water and then transferred to the zone-melting apparatus described in a previous publications to grow large-size aligned polycrystals. The background and ring-heater temperatures were adjusted to make the freezing solid-liquid interface slightly convex to the liquid. The recorded temperature gradient in the vicinity of the freezing solid-liquid interface was around 15°C per cm. The ampule was moved horizontally at a speed varying from 0.4 to 2 cm per hr so that the ring heater would cover the whole ingot length from end to end. A single zone-melting pass was used for the Bi-Te, Sb-Te, and Bi-Sb-Te ingots. Two passes in the forward and reverse directions were carried out for the Bi-Se and Bi-Se-Te ingots. Six passes in the forward and reverse directions were performed for the Bi-Sb-Se-Te ingot. The zone-melted ingots were found to contain several large crystals, with their basal planes (0001) approximately parallel to the growth axis. Samples of bismuth and antimony tellurides coated with a layer of tellurium, and bismuth selenide coated with a layer of selenium, were prepared for comparison in phase identification. These coatings were made by dropping a piece of the zone-melted ingot into some molten tellurium or selenium under argon atmosphere and allowing them to cool slowly to room temperature. The metallographic specimens were prepared by

Jan 1, 1969

By J. E. Lawver, G. L. Samsel

The success of many mineral dressing processes, including froth flotation and electrical concentration, depends largely on knowledge of physical and chemical structures of the mineral surfaces involved. As a general rule solids have surface layers, usually invisible by optical tests, that differ from the substratum. To the mineral engineer, therefore, a knowledge of the surface structures of minerals is of paramount importance. During the past decade one of the most powerful tools in the study of froth flotation mechanisms has been the use of radioactive tracers, but this technique usually cannot give definite information regarding the chemical changes that may or may not have occurred at the surface. The electron microscope and electron diffraction camera can be particularly useful instruments in surface studies.. An election microscope permits much closer examination of surfaces than can be obtained with a petrographic microscope. In certain cases, it is possible to identify trace quantities formed by chemical reaction between flotation agents and mineral surfaces by the use of a single-crystal, reflection electron diffraction camera. This article describes several instances in which these instruments have been valuable guides in mineral dressing research at International Minerals & Chemical Corp. One of the first applications of these techniques employed by International Minerals was in conjunction with the study of electrical concentration of potash ore. The first reasonably successful separation of potash ore was made by subjecting a sample of the ore to a methanol wash. Subsequent tests using tagged 6C14 methanol showed that only a minute quantity of radioactivity was detectable after the methanol-washed sample had been dried and heated to about 300°F. It was concluded that although some methanol had been held to the surface by adsorption, this could not account for the improved electrification because there was no evidence of methanol selectivity with respect to NaCl or KCl. Consequently there must have been some other change in the surface. Carbon replicas* of the mineral grains were made before and after the methanol wash. The replicas were separated from the minerals by dissolving in water. This extraction replica technique is particularly attractive because the specimen can first be used with the electron microscope to observe the general structure of the surface and can be re-used as a specimen for electron-diffraction studies to identify any solvent insoluble material present on the mineral surface." Fig. 1 shows the general

Jan 1, 1960

By Thomas W. Dawson

THE H. C. Frick Coke Co. has used belt conveyers for handling coal for the last eighteen years but, until recently, only for small tonnage and over short distances. The first installations were outside the mines for distributing coal to various parts of plants. A belt conveyer was put in service at Colonial No. 4 Mine in November, 1906, to carry coal from the main hoisting shaft to a storage bin serving two blocks of beehive ovens on the other side of the valley; it was in constant service until the Colonial No. 4 ovens were abandoned less than a year ago. This conveyor was in an overhead gallery that spanned our sidings and yard tracks and the main line of the Pennsylvania Railroad. It was a crude installation, from the viewpoint of present conveyor engineering practice. It had no mechanical feeding device, the coal simply ran through a gate in the side of a bin on to the belt; but one belt on this conveyor lasted eleven years. This conveyor is about 300 ft. long center, to center of pulleys. It operated at a speed of 250 ft. per min. and carried about 400 tons per day. On this basis, the belt life of eleven years means that not over a million and a quarter tons were carried by the belt. While this is not a large tonnage, the cost per ton was much less than by any previous method in use for supplying coal to ovens located at a distance from the main shaft. The next belt conveyor was installed at Bridgeport Mine in 1907. It carried about the same daily tonnage as the first, delivering from the hoisting shaft to a coke-oven bin. Very few data were kept on this conveyor. It also operated until the coke ovens at the plant were put out of blast and the coal taken to the Clairton byproduct plant by river. In 1916, work was started to equip the Bridgeport, Palmer, Gates, and Ronco mines to load their entire output on, the river for transportation to the Clairton byproduct plant, which was then being built. These mines were all operating at that time and had a large area of coal available for river shipment. The Monongahela Railroad was located between the hoisting shaft and the river at each of these plants and,, therefore, had to be crossed at each location to deliver coal to the river.

Jan 6, 1925

By D. P. Pope, T. Vreeland

Observations of dislocations in zinc using Berg-Barrett X-ray micrography confirm the validity of a dislocation etch for (1010) surfaces. A technique for measurement of the depth in which dislocations can be imaged in X-ray micrographs is given. This depth on (0001) surfaces of zinc was found to be 2.5 µ using a (1013) reflection and CoKa radiation. BUCHANAN and Reed-Hill (B & RH) have recently questioned the ability of a dislocation etch to reveal all of the basal dislocations which intersect (1010) surfaces in annealed zinc crystals.' This etch was developed by Brandt, Adams, and Vreeland who conducted a number of different experiments to check its ability to reveal dislocations.2,3 B & RH prepared (0001) foil specimens for transmission electron microscopy from annealed crystals and observed dislocation densities of about l08 cm per cu cm in the foils, while the etch indicated densities of the order of l04 cm per cu cm in their annealed crystals. As this etch has been used in a number of studies of dislocations in zinc, it is of considerable importance to reassess its validity in the light of the B & RH results. The X-ray work reported here was undertaken to check the ability of the etch to reveal dislocation intersections on (1070) surfaces of zinc. The X-ray technique was chosen for this check because it could be applied to the as-grown crystals with a relatively small amount of specimen preparation. We believe that the possibility of accidental deformation in preparation of the bulk specimens is considerably less than that for thin foil specimens suitable for transmission electron microscopy. Unfortunately, basal dislocations are not visible on Berg-Barrett topo-graphs of (1010) surfaces, which are the surfaces on which the etch is most effective. Therefore, a one-to-one correspondence between the etch and X-ray observations could not be made. Basal dislocations near (0001) surfaces have been observed by Schultz and Armstrong4 using the Berg-Barrett technique, but they did not report the as-grown dislocation density observed in their crystals. We have applied the X-ray technique in this study to surfaces oriented from 1 to 2 deg of the (0001) to determine the basal dislocation density, and have compared this density with that observed using the etch on a (1070) plane of the same crystal. The X-ray observations permit determination of the depth in which basal dislocations can be observed under the diffracting conditions used. SPECIMEN PREPARATION High purity zinc crystals are very soft, so a good deal of care must be exercised in the preparation of observation surfaces. As-grown crystals approximately 2.5 cm in diam and 20 cm long were acid cut into 1.25 cm cubes. A thin slab was cleaved from an (0001) surface to produce an accurately oriented reference surface on the specimen. Some of the cubes were examined in the as-machined condition while some were annealed in argon at 410°C for 2 hr. Heating and cooling rates were less than 2°C per min. Some of the specimens were scratched on a (0001) surface with a razor blade to produce fresh dislocations. Approximately 2 mm of material was acid lapped from one face of a cube to produce a surface oriented between 1 and 2 deg from the basal plane and parallel to the [1210] direction. A (1070) surface was also acid lapped. The lap used a 1 to 3 pct solution of HN03 in water to saturate a soft cloth which was backed by a stainless steel plate. The cloth was moved over the crystal surface at a rate of 20 cm per sec while a normal force of about 4 g was maintained between the cloth and the specimen. As-lapped surfaces were examined as were surfaces which were chemically and electrolytically polished after lapping. The small angle between a lapped surface and the (0001) plane was measured to 0.1 deg using a Unitron microgoniometer microscope (the cleaved surface was used as a reference in this measurement). The microscope was modified so that the intensity of reflected light could be continuously monitored on a meter. This modification produced nearly a ten-fold increase in the reproduceability of orientation readings. OBSERVATIONS The Unitron Microgoniometer observations indicated that the lapped surfaces had a terraced structure with the terraces quite rounded and spaced about 0.1 mm in the [1010] direction. The maximum change in slope between terraces was 0.25 deg, indicating a terrace height of about 0.1 µ. A Unitron measurement of the average angle between (0001) and a lapped surface was checked by micrometer measurement of the specimen and found to agree within 0.1 deg. The Berg-Barrett micrographs using (1013) reflections and CoKa radiation5 revealed subboundaries, short dislocation segments, spirals, and loops near the surfaces which were oriented from 1 to 2 deg of the (0001). Micrographs of surfaces prepared by lapping appeared very similar to those of the chemically and electrolytically polished surfaces. The loops and spirals were not extinct in (1013) or (0002) reflections, indicating that they have a nonbasal Burgers vector. Extinctions of the short, straight dislocations indicated that they belonged to an (0001)(1210) system. Fig. 1 is an example of a micrograph which shows a subboundary, and dislocation segments which are pre-

Jan 1, 1970

By D. J. Carney, J. Chipman, N. J. Grant

G. Derge—With the development of this last weapon, there is not much of a chance for hydrogen. It is certainly a very interesting paper, and it gives us more confidence in sampling liquid steel for hydrogen than we have ever had before. This satisfactory work gives considerable confidence to all of the chilled methods of sampling which should be more or less successful depending upon the degree of chilling obtained. J. T. MacKenzie—How do you handle a nonmagnetic specimen in that device? D. J. Carney (authors' reply)—I left that out in going over the analytical procedure. For the 18-8 steel, what was done was to get some iron wire which was degassed. One turn of wire was made around the sample; it was inserted into the analytical apparatus, and that was enough to allow the magnet to pull the sample and drop it in the furnace. Other methods could be devised for this apparatus to do the same thing. This was just a quick method. C. E. Sims—This method of sampling and analysis is very ingenious, and the results obtained attest to a satisfactory degree of accuracy. It was noted in the paper that the samples are satisfactory only when there is a complete absence of pipe. This should be empha- sized, particularly in view of the fact that they are cut off under water. Some reservations are held in regard to the adequacy of the method of sample storage prior to analysis. Cooling on dry ice undoubtedly slows down the rate of diffusion to a marked degree, and it obviously suffices when the analysis is made within a few hours. All of the samples, except some of high-nickel steels, were analyzed within 12 hr. It is still unknown how long this method would be safe. In the work at Battelle Institute, it was impracticable always to start analysis within 12 hr for various reasons. Some samples did not reach the laboratory for several days, and some were held as long as a month before analysis. During this period, they were held over mercury, and the gas evolved at room temperature was collected and analyzed. It should be mentioned that both the mercury and the container must be kept very clean.

Jan 1, 1951

By John M. Hartman

The high temperature of the blast of modern furnaces renders it desirable that the pipe conveying the blast into the furnace crucible shall transmit and radiate as little heat as possible. To accomplish this, the pipe shown in the accompanying sketch was devised and patented. It consists of a slide-valve, leg-pipe, and belly-pipe, which are held together and to the tuyere by a system of levers and links. The slide-valve is superior to the old throttle-valve. The legpipe is formed of two thicknesses of wrought-iron pipe, with a space of half an inch filled in with clay and brick. The belly-pipe is made in the same way as the leg-pipe, and terminates in a globe face to suit the tuyere. The quarter turn is made extra thick, of cast iron, and the cap on the end is lined with clay also. The catches, A, B, C, are merely for convenience in putting the pipe together. The joints D and E are globe faces, and allow the pipe to adjust itself to any angle. The eye-piece is made of violet glass, which cuts off the glare from the bright coals in the furnace and allows a close examination of the interior, so that any water dropping or vapor can be detected. The glass does not become coated with dirt, like mica. Since good running of furnaces is shown by a bright tuyere, it is necessary to have a good eye-piece to examine them. To detach the pipe, a man lifts the weights, the side rods are then slipped off the bell crank under the quarter turn, the link under the belly-pipe is unhooked, and the pipe carried away. The same process is reversed to put the pipe together. The nozzle is changed by taking off the cap, G, drawing the nozzle through the belly-pipe, and inserting another. In this way the change can be made quickly, without taking down the pipe. On the old tuyere pipe bolts with brass nuts were used, which burned up and gave trouble. In other cases key-bolts were used, making it difficult to adjust the pipe. Bolts make too rigid a joint, and there is no provision for movement from contraction or expansion. As the temperature of the blast increases there is more expansion, and where rigid joints are

Jan 1, 1879

By John M. Hartman

THE high temperature of the blast of modern furnaces renders it desirable that the pipe conveying the blast into the furnace crucible shall transmit and radiate as little heat as possible. To accomplish this, the pipe shown in the accompanying sketch was devised and patented. It consists of a slide-valve, leg-pipe, and belly-pipe, which are held together and to the tuyere by a system of levers and links. The slide-valve is superior to the old throttle-valve. The leg-pipe is formed of two thicknesses of wrought-iron pipe, with a space of half an inch filled in with clay and brick. The belly-pipe is made in the same way as the leg-pipe, and terminates in a globe face to suit the tuyere. The quarter turn is made extra thick, of cast iron, and the cap on the end is lined with clay also. The catches, A, B, C, are merely for convenience in putting the pipe together. The joints D and E are globe faces, and allow the pipe to adjust itself to any angle. The eye-piece is made of violet glass, which cuts off the glare from the bright coals in the furnace and allows a close examination of the interior, so that any water dropping or vapor can be detected. The glass does not become coated with dirt, like mica. Since good running of furnaces is shown by a bright tuyere, it is necessary to have a good eve-piece to examine then. To detach the pipe, a man lifts the weights, the side rods are then slipped off the bell crank under the quarter turn, the link under the belly-pipe is unhooked, and the pipe carried away. The same process is reversed to put the pipe together. The nozzle is changed by taking off the cap, G, drawing the nozzle through the belly-pipe, and inserting another. In this way the change can be made quickly, without taking down the pipe. On the old tuyere pipe bolts with brass nuts were used, which burned up and gave trouble. In other cases key-bolts were used, making it difficult to adjust the pipe. Bolts make too rigid a joint, and there is no provision for movement from contraction or expansion. As the temperature of the blast increases there is more expansion, and where rigid joints are

Jan 1, 1879

By O. D. Sherby, J. E. Dorn, C. D. Wiseman

MCLEAN' has shown that the total strain obtained during creep of aluminum polycrystals arises exclusively from the mechanisms of 1) microscopically observable slip, 2) subgrain tilting, and 3) grain boundary shearing. Extensive analyses, however, suggest that the high temperature creep of metal polycrystals is controlled by a single thermal activation process."" These somewhat contradictory observations might be reconciled if it could be shown that the activation energies are identical for each of the mechanisms isolated by McLean. Such identity of the activation energies, of course, would demand that the same unit process controls the functioning of each individual mechanism. Under these conditions the activation energies for creep of single metal crystals and polycrystalline aggregates and for grain boundary shearing should be identical. This paper is primarily concerned with the possible identity between the activation energies for high temperature creep of single crystal and polycrystalline metals. In addition, comparisons will also be made between the activation energies for creep of single crystals and polycrystals with previously reported activation energies for grain boundary shearing.0"8 Materials and Techniques The same high purity aluminum, lead, and tin were used in the creep tests for single crystals and polycrystalline aggregates. Single crystals of aluminum and tin were prepared by the strain-anneal technique, whereas lead single crystals were prepared by growth from the melt. The tensile creep stress was maintained constant by Chalmers-Andrade parabolic-type lever arms. Strains were measured to &0.0002 in. per in. with rack and pinion type extensometers, and temperatures were maintained to within & 0.2"C of the reported values by mercury-thermoregulated resistance-heated silicone oil baths. The previously reported unambiguous technique for determination of the activation energy for creep was employed throughout this investigation.' ." It involves periodic abrupt small changes in temperature during the course of creep, accomplished by rapidly replacing one creep bath at temperature TI by a second bath at T,. The abrupt change in creep rate from i, to & attending the abrupt change in temperature is due exclusively to the change in temperature, since both the stress and the substructure are identical the instant before and the instant after a change of temperature. Therefore, all other factors being identical where AH is the activation energy for creep and R is the gas constant. Results Typical examples of the creep rate vs creep strain data during temperature cycled creep tests of single

Jan 1, 1958

By Wallace Ralston

The East Texas district includes the northeast 38 counties of the State of Texas. It still remains one of the most important oil-and-gas-producing areas of the United States, since it includes within its boundaries the large East Texas field. Other fields of importance are: Van, Rodessa, Talco, Cayuga, Long Lake and Sulphur Bluff. Production is from the Nacatoch, Blossom, and Woodbine of the upper Cretaceous and the Paluxy and Glen Rose of the lower Cretaceous. Of these, the Woodbine is the most important, since it is the producing horizon iri the East Texas field. Fields East Texas Field.—There were 2471 oil wells, 1 gas well and 84 failures completed during the year of 1936 in the East Texas field; that is, 1565 fewer than in the year of 1935. The total number of producing wells is now 22,031, of which 50 are temporarily shut down; 18,435 wells flowing their production; 3150 pumping; 293 on gas-lift, and 82 operated by other methods. This shows an increase of 1642 wells on artificial lift over Jan. 1, 1935. The average daily salt-water production is estimated at 42,700 bbl. from 2327 wells—an increase of 1201 wells over the year of 1935. The field is now drilled to an average density of one well to 5.85 acres. Average bottom-hole pressure has dropped from 1193 Ib. to 1168 lb., approximately 1 lb. drop for each 6,600,000 bbl. of oil produced. During the month of December 1936, the estimated daily average production of illegal oil had dropped from 20,500 bbl. in December 1935 to 7500 bbl. The commercial gas production is of minor importance in the East Texas field, and figures for the amount of gas taken from the field are not available at the present time. Talco Field, Titus and Franklin Counties.—The discovery well was drilled by Housh, Thompson et al. on the C. M. Carr tract and completed in March 1936, as a pumping well making 552 bbl. per day of 24' gravity oil. This well was first completed at a total depth of 4208 ft., the top of the sand being 4190 ft. Later it was deepened to 4260 ft., which increased the production from 552 to 725 bbl. per day. This field is producing

Jan 1, 1937

By G. Nabi, W-K. Lu

Cylindrical specimens of natural dense hematite were reduced to magnetite at atmospheric pressure in H2-H2O mixtures of known composition over the temperature range 1084° to 1284°K. The rate of reduction was measured by the rate of movement of the interface between hematite and magnetite. The diffusion of gases through the gaseous boundary layer, the magnetite layer, and the interfacial chemical reaction were all considered in the interpretation of experimental data. The mass transfer coefficient through the boundary layer was calculated using accepted correlations. Values of the chemical reaction rate constant and the diffusivity of hydrogen in the magnetite phase were determined. THE present investigation is concerned with the reduction kinetics of natural hematite to magnetite by H2-H2O mixtures in the temperature range 1084" to 1284°K at atmospheric pressure. This reaction is the first step in the series of topochemical reactions in the process of reducing hematite to iron. Kinetic information of the simple steps such as hematite-magnetite transformation is necessary in order to have a better understanding of the complex processes of hematite reduction in iron-making. It also has direct industrial significance because magnetic roasting is one of the most important methods in benefication of lean ore.&apos; Although many technical papers have been published on the process of magnetic roasting and iron oxide reduction, very little information is available in the literature concerning the fundamental nature of hematite reduction to magnetite by reducing gases. Hansen et al.2 reduced the dense synthetic pellets of high-purity oxide in CO-CO2 mixtures and determined the reaction rate by weight-loss method. They were able to interpret most of their results by applying the interfacial area control theory developed by Mckewan.3 In contrast, Wilhelm and St. Pierre,4 who studied reduction of hematite to magnetite in H2-H2O mixtures by weight-loss method, stressed that the resistance of the porous magnetite layer to the diffusion of gases cannot be neglected in consideration of the overall reaction rate. In the present study the contributions of interfacial chemical reaction, diffusion of gases through the magnetite phase, and the gaseous boundary layer to the overall reaction rate will be considered. APPARATUS AND PROCEDURE Hematite Specimens Preparation. Natural hematite ore from Vermillon range of Northern Minnesota was selected for the present investigation because of its high purity and thermal stability. Chemical analysis of five samples gave the following average values: 67.52 pct total iron (96.62 pct Fe2O3, 0.28 pct FeO, 0.03 pct metallic iron), 2.53 pct SiO2, <0.07 pct MgO, 0.03 pct CaO, 0.05 pct combined mixture, 0.07 pct loss on ignition, and 0.34 pct other. Cylindrical specimens of 0.93 cm in diam and 2.7 cm in length were drilled from slabs of ore with a water-cooled diamond core drill. These specimens were heated to 1000°C and furnace-cooled. Specimens with silica pockets developed large cracks. The uncracked specimens were heated a second time, and their surfaces were carefully examined with a microscope. Those with hairline cracks or surface inhomoaenitv-- were rejected. Preparation of H2-H2O Mixtures. H2-H2O mixtures were prepared by the combustion of H2-O2, mixtures in a pyrex glass chamber in the presence of a catalyst. Alumina pellets coated with palladium, supplied by Englehard Industries, were used as the catalyst. Purified grades of hydrogen and oxygen were used which were repurified by usual techniques. Hydrogen before entering the combustion chamber was passed through an activated alumina H2O absorption bulb, with copper turning at the top. The cover of this bulb was not made pressure-tight so that any pressure development in the hydrogen line would cause the cover to blow off and also the copper turnings would act as a flame arrester in the case of a flashback from the combustion flame. Oxygen flow rates were measured with a bubble flow meter after purification with 1 pct accuracy. Hydrogen flow rates were measured by "precision wet test meter" and the amount of unburnt hydrogen was accurately measured by a bubble flow meter, after condensing water vapor in the gaseous stream. The Pyrex glass bulb contained concentric Vycor glass tubes as shown in Fig. 1. Oxygen was prevented from diffusing into the hydrogen line by threading platinum wire through pores at the combustion end of gas inlet tube. The glass bulb was heated with a Kanthal heating wire pasted in asbestos paper. The surface temperature of the bulb was measured with a thermocouple and adjusted to remain at approximately 350°C. The gaseous reaction chamber also served as a preheater for gases to avoid thermal segregation. The following sequence of operation was adopted. 1) Nitrogen was passed through the outer concentric tube to purge the catalyst bulb of oxygen. 2) Hydrogen was introduced through the inner tube until a steady flow was obtained. 3) Oxygen was then introduced into the nitrogen stream passing through the outer tube. 4) When combustion had commenced and a flame was visible over the platinum wire, the N2 was turned off.

Jan 1, 1969