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By R. L. Grunes, F. K. Kies, C. D&apos, Antonio

THE several studies concerned with the annealing of thin nickel films have largely been restricted to films of a single thickness.1-4 It is well-known, however, that both physical and mechanical properties depend upon film thickness.5, 6 The strength-thickness relations found in vapor-deposited nickel films in the annealed and as-deposited states, as an example, are at least partially due to the density and arrangement of imperfections within the films.7, 8 For these reasons, the annealing characteristics of thin nickel films as a function of thickness were investigated. Electrical resistance was chosen to monitor annealing behavior since resistance changes are partially dependent upon defect structure. In addition, the equations predicting film resistivity as a function of thickness are already available.9, 10 Further advantages afforded by electrical-resistance measurements are its adaption to continuous readings during annealing and its relative simplicity. Nickel films were vapor-deposited, at average rates of 60Å per sec, on Vycor substrates held at room temperature in vacuums of about 10-5 torr. Afterwards, deposition-thickness measurements were made using a multiple-beam interferometric technique. A more detailed description of deposition procedures and the interferometer appear elsewhere.7, 8 The four-probe method was employed in measuring electrical resistance since this technique measures film resistance without contributions from lead wires and contacts. Resistance measurements were made before, during, and after annealing to temperatures of 700°C under vacuums of approximately 10-4 torr. Measurements were made every 25°C or more often when necessitated by unusual resistance changes. Cooling and heating rates were maintained at approximately 5°C per min. Typical resistivity vs temperature curves are shown in Figs. 1 through 4. It is apparent from these

Jan 1, 1965

By Frank E. Woolley, Robert D. Pehlke

Jan 1, 1965

By Forrest T. Moyer

INJURY experience in the metal and nonmetal mineral industries during 1964 was better in rates of occurrence but worse in severity rates than in 1963. The frequency rate of injuries per million man-hours was improved at metal mills, nonmetal mines, and sand and gravel operations, and was virtually unchanged at metal mines; however" the rate of occurrence of work injuries at nonmetal mills, stone operations, nonferrous reduction and refining plants, and slag plants was higher than in 1963. The severity rate of injuries during 1964, data for which are presented for the first time in this chapter, was better at metal mills, nonmetal mines, stone operations, and slag plants. However, the severity rate was worse at metal mines, nonmetal mills, sand and gravel plants, and nonferrous smelters.

Jan 1, 1965

By William D. Klopp

A study was conducted of the tensile and creep properties of are-melted and electron-beam-melted tungsten over the temperature range 2250° to 4140°F. The tensile and creep strengths vary with pain size, the finer -grained materials being stronger. The activation energy for transient creep at 2250° to 3500°F is 95,000 cal per (g)(mole), while that for steady creep at 3300o to 4000°F is 141,000 cal per (g)(mole). At 2875o to 3300°F the apparent activation energy for steady creep decreased with decreasing temperature. It is suggested that cross slip is rate controlling during transient creep, while dislocation climb is rate controlling during steady creep above 3300° F. ALTHOUGH considerable data have been generated on the high-temperature tensile properties of powder-metallurgy tungsten,1 relative few data have been published on the properties of are-melted2 or electron-beam melted tungsten.3 Furthermore, the available data show a fairly large amount of scatter at high temperatures. The effects of structure and purity have not yet been defined, aside from observations that high-purity electron-beam (EB)-melted tungsten3 and single-crystal-plasma-flame tungsten4 are weaker than less pure powder-metallurgy tungsten. The creep behavior of powder-metallurgy tungsten has been studied, but no data are available on the creep behavior of tungsten consolidated by melting. Green5 found that powder-metallurgy tungsten exhibited linear creep at 4082° to 5072°F with an activation energy of 160,000 cal per (g) (mole). The similarity of this activation energy to that of 153,000 cal per (g)(mole) for volume self-diffusion6 suggests that recovery of strain hardening by dislocation climb is rate controlling in this temperature range. In studies at 4800°F, Sutherland and Klopp7 concluded that grain size significantly affected the creep behavior of commercial powder-metallurgy materials. This grain-size effect was suggested by sherby,8 although the opposite relation had been reported for aluminum.' The purpose of the present study was twofold: first, to provide baseline data on high-temperature tensile and creep properties of are-melted and EB-melted tungsten for concurrent tungsten alloy studies, and, second, to determine the phenomenolo-gical effects of structural and purity variables on the high - temperature mechanical properties of tungsten. EXPERIMENTAL The are-melted tungsten materials were prepared by melting sintered 1-1/4-in.-diam electrodes into 2-1/2-in.-diam by 5-in.-long ingots. The are-melting facility has been described previously.' Eight ingots were melted, machined, and hot-extruded at

Jan 1, 1965

By Charles E. Whieldon

Data on the oilfields in Mahoning, Columbiana, Carroll, Jefferson, and Harrison Counties, Ohio, were collected from scattered sources and compiled to make the information readily available to operators who may be interested in conducting secondary-recovery operations in the area. General geology, oil production, oil-productive acreage, core data, reservoir calculations by townships, and miscellaneous data and reference material are presented.

Jan 1, 1965

Jan 1, 1965

By Thomas C. Wilder

Jan 1, 1965

By Hugh M. Roberts

In the spring of 1915, then a 30-year old geologist in the employ of the E. J. Longyear Co., of Minneapolis, Minn., I accompanied prospectors to ex- amine outcrops of supposed nickel ore situated a mile or two in from the shore of a lake in the Kenora district of northwestern Ontario. The deposit proved to be bog iron ore containing traces of nickel. We were stormbound there for three days, a circumstance which gave rise to a tale that was told at our fire one night. It seems that Sandy and Jock, two prospectors, were crossing the bay of a large lake in a canoe. They were bucking headwinds; the waves grew higher. Jock called out from the stern, "Sandy, can ye na pray a little." Sandy pressed his knees a little closer into the bow and, between strokes of his paddle, sought for words, which came haltingly, "Save us this time . . . Oh Lord . . . and we promise . . ." when Jock, peering through the spray sang out, "I would na commit yourself, Sandy, I think I see lond ahead."

Jan 1, 1965

By D. M. Kehn

A method has been devloped for chromatographic analysis Of the vapor and liquid phases Of a a system containing methane to components having 20 or more carbon atoms. The method uses a windowed equilibrium cell in which volumetric phase behavior of the system can be observed accurately and from which small samples of gas or liquid can be withdrawn for analysis. Analyses are made using two chromatographs, one for the lighter and one for the heavier components in a sample. Combination of the two analyses yields a detailed analysis of the gas or liquid sample. The complexity of the condensate heavy ends is evident from the chromatograms of these fractions, and the predominance of the paraffin hydrocarborn serves as a useful marker in interpreting the chromatograms. The K-values obtained in this analytical method are presented for a high-pressure condensate system and predict closely the observed volumetric behavior of the system. INTRODUCTION Quantitative analysis of hydrocarbons from natural gas reservoirs is necessary for several reasons—to calculate the amount of sales gas produced, to calculate the amount of natural gasoline produced, to plan a liquid recovery system, or to calculate the potential economic value of a reservoir produced under one or more of several different conditions. Analysis of natural gas fluids produced to the surface consists of identifying and computing the mol fraction of each component of the mixture. Although methane is the predominant component, varying amounts of ethane, propane, butane, pentanes and heavier components are also present. Materials containing up to 30 carbon atoms occur in amounts which decrease with increasing molecular weight. However, the quantities of components in the 20 to 30 carbon atom range are usually so small that their importance is negligible, and they are undetect-able in natural gas by ordinary analytical methods. All the components up to those having 20 carbon atoms may sigsficantly affect phase behavior, however. Commonly, only the methane-through-pentane fraction is analyzed quantitatively for each component, while components heavier than Pentane are lumped and repored as "hexane- plus". Expensive, tedious techniques are required for analysis of this fraction. Consequently the detailed analyses needed for prediction of reservoir behavior are usually undertaken only when major gas fields are being developed. The need for complete analyses of condensate systems is apparent when it is recalled that most gas fields are produced by pressure depletion. As the pressure declines, some of the heavier hydrocarbons are lost as liquids which are in the reservoir. In many instances the amount of liquid in equilibrium with the gas phase at high pressure constitutes only 1 or 2 mol per cent of the total system. Flash calculations generally must predict the actual amount of liquid with an accuracy of a few per cent in order to be useful. This retrograde condensation has been understood for years, but accurate correlation methods to permit quantitative prediction of phase behavior in the retrograde region are not presently available. The increasing importance of natural gas has made accurate prediction of phase behavior and composition of produced natural gas streams an economic necessity. The work reported here was undertaken to provide a rapid, economical method for obtaining the vapor-liquid equilibrium information needed to predict accurately the composition of the fluids produced from a gas reservoir throughout its life. TO develop this method, a pressure cell equipped with windows was designed and built for observing the volumes of liquid and gas present at reservoir pressures and temperatures. Use was made of established chromatographic methods for rapid and detailed analysis of both phases. This paper describes the equipment and techniques developed for obtaining vapor-liquid equilibrium data, presents the results of analyses of a condensate system, and indicates the usefulness of these data in predicting hydrocarbon phase behavior. DESCRIPTION OF EQUIPMENT USED The equipment used in obtaining the required information on phase behavior and the complete analysis of hydrocarbon mixtures through C, will be described first, followed by a discussion of the operation of the equipment. It will be helpful, however, to consider first a brief outline of the technique used. A sample of separator gas and liquid is charged to the windowed cell (see Figs. 1 and 2) where volumetric equilibrium phase behavior at reservoir pressures and temperatures can be determined. Then samples of the coexisting phases are withdrawn. The methane-through-pentane fraction is analyzed with a chromatograph equipped with a hot-wire detector, and the pentane-plus fraction is analyzed with a second chromatograph equipped

Jan 1, 1965

By Walter Kahn

Increasing consideration is being given to simplifying traditional methods of tracing pipelines and maintaining required temperatures of stored fluids. Because of their reduction in capital costs, virtual elimination of maintenance. ease of control and "cleanliness"; interest in electrical techniques has accelerated. 1,2 Resistance cable and other heaters have been given some attention. but less well known in the recent introduction of thermal conductive coatings. This paper is addressed to the use of thermal conductive coatings for heating fluid-transport piping and storage tanks. Emphasis will be given to the simplicity, efficiency, and versatility of design and application which their unique properties further contribute to the general economics of electrical heating.

Jan 1, 1965

By M. N. Shetty

LARGE copper whiskers (-100 p) of 11111 orientation were tested in a floor-model Instron testing machine, at liquid nitrogen temperature. (Testing methods will appear elsewhere.) Whiskers deformed by twinning after some initial deformation. A load-elongation curve at the onset of twinning is reproduced in Fig. 1. Twinning was confirmed by taking a back-reflection Laue picture, using a slit colli-mator, which showed distinct splitting of reflections. The tensile stress reached just before twinning is about 1.4 x 107 g per sq cm (-7.0 x106 g per sq cm—resolved shear stress) which drops to 1.2 x107 g per sq cm (-6 x 106 g per sq cm—resolved). This twinning stress is about five to ten times larger than the value for bulk single crystals of copper deformed at 77°K (-106 g per sq cm—resolved). Twinning models based on Cottrell-Bilby's pole mechanism are discussed in detail by Venables.' In the present work a mechanism based on the idea of failure of a Lomer-Cottrell barrier by recombination will be proposed. An L-C barrier may fail either by recombination or by dissociation.3 Fig. 2 provides the necessary information. It shows that the stress necessary to break such a barrier is about 1.8 x 107 g per sq cm by recombination and 4 x 107 g per sq cm by dissociation at 77°K. The twinning stress reached by whiskers is comparable to the stress level required for failure of an L-C barrier by recombination. (Stroh himself points out that his calculations should not be taken too literally.) We consider a segment of the L-C dislocation which has recombined (AB in Fig. 3) over a length to form the total dislocation which then glides in the

Jan 1, 1965

By M. Copeland

Phase relations of gadolinium alloyed, up to 40 weight-percent (wt pct), with AISI 304-type stainless steel were established. Body-and face-centered cubic iron-rich solid solution phases and several intermetallic gadolinium-containing compounds of variable composition that approximated the formulas Fe9Gd, Ni7Gd2, Ni3Gd, Fe2Gd, NiGd, and NiGd3 were identified. The intermetallic phases Fe9Gd and Ni7Gd2 were noted to melt at about 1,080° C at about 0 to 2 wt pct gadolinium. The melting temperature of Fe9Gd increased with increas-ing gadolinium content to a plateau at about 1,230°C and 30 wt pct gadolinium, and the melting point of Ni7Gd2 decreased to a plateau at 900° C and 30 wt pct gadolinium where Ni3Gd, NiGd, and Fe2Gd coexist. Body-centered cubic iron solid solution was stable from 1 to 2 wt pct gadolinium to higher contents, 30 wt pct gadolinium or possibly more, and face-centered cubic iron up to 12 wt pct gadolinium below 1,200° C. The stability of these phases above 1,200° C was not resolved except for the mel points. A limited number of fabrication variables as well as mechanical and corrosion properties of alloys containing up to 5 wt pct gadolinium were studied. Equilibrating and forming operations were best conducted at about 940° to 1,080° C. Some variability in the yield and tensile strengths of alloys was noted; however, there was a continual decrease in ductility and impact resistance with increasing gadolinium contents. The resistance of gadolinium alloys to corrosion in water at 354° C was about the same as stainless steel.

Jan 1, 1965

By Waugh D. M

investigations have been undertaken into the flow characteristics of mineral slurries from a number of Australian metallurgical plants including Mount Isa Mines Ltd., North Broken Hill Ltd., and Broken Hill South Ltd. Experimental equipment installed for this work included facilities for continuous recording of flow rate and pressure drop and detection of sedimentation.Although the method has subsequently been described in published literature, it is believed that the investigations included the original application of a method for correlation of the flow rate and pressure drop data. This method depends on solving by graphical methods the values of the constants k, and c in the relationship EQUATION 1 where D is pipe diameter; ?P, pressure drop; L, length; and V, mean linear velocity. Discussion of this correlation also reveals why sedimentation velocity does not necessarily vary greatly with pipe diameter.INTRODUCTIONIn order to design pumps and pipeline installations for a Newtonian fluid, measurements of the fluid's density and viscosity in any of a number of instruments are sufficient. Substitution of these values in well known equations to calculate Reynolds numbers and subsequent correlation to determine friction factors are all that is required for engineering specification.As a result of work during the last decade, particularly that of Metzner and Reed (1955) and Dodge and Metzner (1959), it is now possible to design for homogeneous non-Newtonian fluids using relatively simple instrumental measurements.These methods can sometimes be applied to thick slurries which behave as if homogeneous. However, for the...

Jan 1, 1965

By Jack G. Crump

Nuclear radiation systems for gauging solids content in process slurries and level in crushers has demonstrated acceptance in ore processing. The use of nuclear radiation for moisture analysis of bulk materials is presently receiving acceptance in beneficiating and agglomerating processes. On the horizon is the use of nuclear activation methods for continuous, qualatative and quantitative analysis of concentrate. The common characteristics of these uses of radiation is the non-contacting nature of the measurement. Unquestionably, this is the dominant reason for acceptance of nuclear methods in level and slurry-gauging. Moisture activation analysis of a product using nuclear methods retain this advantage. However, and: more importantly, they offer new solutions to old problems. The nuclear method in addition to being non-contacting, is non-destructive and provides a continuous measurement of the process variable. The system responds: to the fundamental makeup of matter, mass and elemental composition, not to secondary properties such as temperature, resistivity, or dielectric constant. Measurement is a volume rather than a surface phenomenon, thus the results can provide a truer pricture of the measured variable.

Jan 1, 1965

By C. F. Giermak

Over a considerable period of time great interest has been shown in selective dry concentration of fine ferromagnetic particles, although it is only recently that new permanent magnetic materials have been made available to permit building of such permanent magnetic separators. It is well known that the conventional drum separator does' not efficiently separate fine materials. The centrifugal force on any drum acts in accordance with the particle size and gravity, which may beat varying magnitude-.opposite to the magnetic force, especially when the material is not closely sized. The Magnetic-Mechanical Separator (MMS) is designed for the concentration of fine, unsized magnetic materials where the percentage composition of magnetics to nonmagnetics, or the nature and texture of the materials, is such that its unique agitation and shake-out action with no centrifugal force provides greater efficiency than is obtainable by conventional magnetic separation equipment. This machine consists of a complete double belt conveyor unit with a premagnetizing Axial Pole Agitating Pulley at the feeding end of the lower conveyor belt and a special agitating concentrator magnet above the lower belt of the upper conveyor.

Jan 1, 1965

By Warren E. Morrison

Stimulated by 4 years of continuous economic growth without inflation, demand for energy in the United States reached an alltime high in 1964. Total value of production of goods and services (gross national product--GNP) for the year was $629 billion, an increase of 6.8 percent from 1963. Allowing for price changes based on 1958 dollars, the gain in real terms was 5 percent. In 1964 the Federal Reserve Board Index of Industrial Production stood at 132, a rise of 6.2 percent. With the impetus provided by personal income and corporate tax reductions during the year, aggregate wages, profits, and consumption reached record levels. Even the persistent balance of payments problem improved. Against this background the national consumption of commercial energy increased 4.2 percent. Energy needs continued to be met largely from domestic resources with imports, mainly crude petroleum and refined petroleum products, accounting for but 7 percent of the total. Mineral energy resources, namely gas, coal, and petroleum, contributed 96 percent of the input of energy into the economy during the year. The remaining 4 percent came from hydropower and nuclear power.

Jan 1, 1965

By S. R. Goodman, Hsun Hu

A study has hem made of the formation of annealing textures in an 18-8 austenitic stainless steel (Type 304L) from various deformation textures obtained by rolling at different temperatures. When the deformation texture is a mixture of the ferritic type and the brass type owing to the pres -ence of both martensitic ferrite and retained aus-tenite in the specimen, recrystallization takes place by the growth of the existing austenite phase. In a previous report,' it was shown that the rolling texture of austenitic stainless steel (Type 304L) changed gradually from the brass type to the copper type with increasing temperature of deformation above 200°C. These changes are similar to those in high-purity silver2,3 and electrolytic copper;4 a brass-type texture is favored at low rolling temperatures, whereas a copper-type texture is favored During the course of rolling -texture transition from the brass type to the copper type, the subsequent recrystallization textures change accordingly. The orientation relationship between the annealing textures and the various rolling textures, being consistent with previous observations on various fcc metals, can be described as [Ill] rotations of approximately 25 to 40 deg. Carhide precipitation may influence the annealing textures. at high rolling temperatures. Furthermore, the annealing textures in high-purity silver5 and electrolytic copper4 were found to depend entirely on the prior deformation texture. From a copper-type rolling texture a strong cube texture will form upon recrystallization, whereas from a brass-type rolling texture the annealing texture will be quite different from the cube orientation. In an earlier comm~nication,6 the formation of a strong cube texture in 18-8 austenite stainless steels (Types 304 and 304L) was reported briefly by the authors. The present paper constitutes the results of a complete study of the annealing textures obtained from a

Jan 1, 1965

By Lawrie D. C

Finely ground beryl was decomposed by mixing with ground limestone and soda ash and heating at 900°C for 4-6 hr. The sintered mater:al was then crushed and leached by boiling under reflux with 5N sulphuric acid for up to 4 hr. The liquor containing Be, AI, Fe and other elements as sulphates, was separated from the residue which consisted mainly of silica and gypsum, either by filtration or bydecantation washing.The clarified leach liquor was first treated to remove Fe+++ by contacting with a primary amine-kerosene solution in 2 countercurrent stages. The iron free liquor was then passed to a 4-stage counter-current extraction unit where it was contacted with O·5M di- (2 ethyl hexyl) phosphoric acid (EHPA) in kerosene. Under the operating conditions, 99 per cent of the Be and 7 per cent of the Al was extracted.The Be and Al were stripped from the organic phase by sodium hydroxide solution of suitable concentration to form soluble "beryllate" and "aluminate" respectively. Most of the Be was subsequently precipitatedas Be(OH)2 by heating the alkaline solution to 90°C, the Al remaining in solution. After filtration and washing, the Be(OH)2 could be ignited directly to BeO at about 1000°C or used as a feed to further purification stages if required.A small counter-current extraction unit was operated continuously using liquor derived from the sintering and leaching stages. Dataobtained in batch laboratory tests were confirmed. A product obtained by ignition of the washed "beryllate" precipitate contained more than 99 per cent BeO.INTRODUCTIONIn 1958 an investigation was commenced into the recovery of beryllium oxide from beryl, as part of a programme to utilize mineral resources of South Australia. A survey of the literature indicated that little work had been done on direct solvent extraction of beryllium from aqueous liquors, so it was decided to apply the experience gained in this field in uranium processing to the current problem.Preliminary extraction tests on solutions of beryllium...

Jan 1, 1965

By G. Krauss, W. Pitsch

The fine structure of the bcc martensite formed in an Fe-33 wt pct ATi single crystal of arrstenite is sho~on by transmission electron microscoPy to consist of combinations of transformation twins, stacking faults, deformation twins, and regular arrays of parallel screw dislocations. These structures constitute evidence for the multiple lattice-invariant deformations which operating during the formation of martensite could produce the real habit-plane scatter measured by a two-surface analysis of the plates formed in the single crystal of this investigation and reported in the literature for other Fe-Ni rnartensites. CRYSTALLOGRAPHIC theories1,2 of martensitic transformation show that the habit plane of martensite in a parent lattice is dependent in part upon an inhomogeneous distortion or lattice-invariant deformation which takes place on a fine scale within a martensite plate during its formation. Several recent theoretical papers3,4 have addressed themselves to an analysis of a wide variety of conceivable lat-tice-invarient deformations and the habit planes which they produce, while experimental investigation have been concerned with either the measurement of habit planes or the description and identification of the martensitic fine structure which reflects the nature of the lattice-invariant deformation operating during transformation. In Fe-Ni alloys with subzero Ms temperatures, the group of alloys with which this paper concerns itself, habit planes have often been found to scatter an amount greater than might be expected from possible experimental errors,5-7 and fine twinning has been identified as a major constituent of the fine structure of martensite.8-11 It has been suggested3,4 that more than one type of invariant shear occurs during martensitic transformation. This possibility has been experimentally supported12,13 by the observation of both dislocation configurations and twinning in a single martensite plate. The purpose of this paper is to report additional evidence for multiple lattice-invariant deformations in martensite and so to account for the real scatter in the habit planes of the martensite plates formed in Fe-Ni alloys. EXPERIMENTAL PROCEDURE The Fe-Ni single crystal was produced by pulling a high-purity iron and nickel charge through a single-crystal vacuum furnace in an alumina crucible. The crystal was double-melted to promote homogeneity and to increase its size by further additions on the second pass. In its final form the crystal was 4 cm in diam and 5 cm long. The nickel and carbon contents were analyzed at 32.9 and 0.006 wt pct, respectively. The austenite of this alloy first transformed to martensite by bursts at about -120°C, and, to preserve as much of the austenite as possible, all transformation was performed just below -120°C. Some observations were made on transformed samples which had been heated for 2 min at 340°C. It is assumed that the features of the martensite of these samples, Figs. 1 and 4, are the same as those of the as-quenched martensite. Orientation of the crystal by X-ray diffraction established 10.735 0.609 0.3161? as the axis of the crystal, an orientation that was checked within 2 deg by neutron diffraction. Further checks by electron diffraction of samples cut normal to the axis confirmed this orientation within the larger limits of error inherent in electron diffraction of thin foils. The X-ray orientation was the one used for the two-surface analysis of the martensite habit planes. A two-surface analysis was performed on the quadrant of the single crystal which had been oriented by both X-ray and neutron-diffraction techniques. Photomicrographs at X50 were made on two surfaces along an edge 2 cm long. Fiducial marks and the fact that many of the plates were almost completely surrounded by retained austenite made good matching of individual plates on two surfaces possible. The habit-plane trace on a surface was taken as the best line parallel to the long axis of a plate. A measure of the accuracy afforded by this criterion was provided by a family of very large plates which appeared at intervals along the entire 2 cm length of the edge. The plates all had habit-plane traces within 2 deg of one another. Many of the plates did not show midribs and, therefore, the use of midribs7 to represent habit-plane traces was not feasible in this investigation. The over-all experimental accuracy is estimated to be better than ±2 deg. Samples for transmission examination in a Siemens Elmiskop I at 100 kv were prepared by cutting 2-mm-thick discs from the single crystal, removing about 0.5 mm by chemical polishing,14 trans-

Jan 1, 1965

By N. A. D. Parlee, I. D. Shah, W. C. Phelps

THIS note reports on a continuation of a program on the thermodynamics of Fe-S-X systems in the "steel-burning" temperature range begun by Bock, Barloga, and parlee.' Small coils of 0.039-in.-diameter pure iron (Ferrovac-E) wire were equilibrated with Fe-S-0 melts in ingot iron crucibles under argon at 1324°C in the assembly shown in Fig. 1, the lower part of which was heated in a large Globar furnace. Fig. 1 shows (R) the coiled iron wire sample, (M) the Fe-S-0 melt prepared from desired proportions of ferrous sulfide and ferric oxide, (K) the iron crucible, (I) a mullite guide tube, (J) an alumina crucible, (L) alundum sand, (N) crushed mullite, (Q) hollow cylinders of K30 brick, (C) a steel rod, (B), (El, (F), (G), (P), and (O), details of brass water-cooled head, and (H) a mullite tube 2-3/4 in. ID and 26 in. long. The rod (C) bearing the sample could be removed at will and be replaced by a tube for sampling the melt, or by a thermocouple for comparing the melt temperature with a control thermocouple not far from the 2-3/4-in. mullite tube. After equilibration the iron coils were treated with acid to remove the outer layer of metal and then they were analyzed for sulfur by a standard combustion method. The melt samples were analyzed for oxygen by a variation of Lander's2 hydrogen-reduction method for mattes, and for sulfur by the ASTM combustion-iodometric method NO. E 30-47. When the results of some forty-two runs were examined it was found that the sulfur and oxygen contents of the equilibrated melts showed good consistency, in that the plotted compositions fell along the smooth curve shown in Fig. 2. The points on this curve represent the experimental compositions of melts in equilibrium with ?-iron (Fe-S-0) solid solutions. These solid solutions are saturated with sulfur and oxygen with respect to the melt and therefore have the same sulfur and oxygen activities as the melt. The curve drawn through the points therefore delineates the ? liquidus. It falls in such a position as to roughly confirm the liquidus curves of Hilty and crafts3 at 1200" and 1300°C which are

Jan 1, 1965