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Coal Division Industrial Minerals Division Minerals Beneficiation Division Mining, Geology and Geophysics Division Council Will Mitchell, Jr, Chairman (MBD), Kenneth L Cook, Vice-Chairman (MGGD). Edward L Clark (MGGD), Raymond B Ladoo (Ind Min Div), Sandford S Cole (Ind Mm Div), Norman L Weiss (MBD), C T Hayden (Coal), H F Yancey (Coal), Clayton G Ball (MED), P De Bruyn (MIED), Arnold Buzzalini, Secretary, AIME, 29 West 39th Street, New York 18, N Y Mining Branch Advisory Committee Will Mitchell, Jr, Chairman, Grover J Holt, J B Morrow, J L Gillson, Edward G Fox, S S Cole, Roger V Pierce, Norman L Weiss. H C Weed. J R Van Pelt

Jan 1, 1956

By E. N. Mazza, H. S. Kalish

The effect of sintering types 302, 3028, and 430 stainless steel powder compacts in hydrogen and dissociated ammonia was investigated. It was found that sintering in dissociated ammonia resulted in as much as 0.5 wt pct increase in the nitrogen content of stainless steel even though the dissociation of the gas was complete. Sintering in hydrogen, on the other hand, reduced the nitrogen content of the stainless steel to less than 0.01 wt pct. In the case of the 302-type stainless steel, the low nitrogen content resulted in a material that was largely ferritic, whereas the high nitrogen content rendered the material fully austenitic. Sintering in dissociated ammonia resulted in lower density, generally lower tensile strength, less ductility, and higher hardness than sintering under equivalent conditions in hydrogen. The reduction of oxides on both stainless steel and iron particles was found to be effected by hydrogen partial pressure in the sintering atmosphere. Compacting pressure was found also to effect oxide reduction during sintering. DISSOCIATED ammonia often is used as a substitute'.' for hydrogen in sintering and in annealing, since economic advantages sometimes can be obtained by such a substitution. In addition, anhydrous ammonia contains very little impurity. Thus, dissociated ammonia gas is very dry whereas tank hydrogen often must be freed of oxygen and water vapor prior to use in many applications. The sintering of stainless steel powder compacts as well as bright annealing is well recognized as requiring a hydrogen atmosphere and for the foregoing reasons dissociated ammonia is frequently substituted. It has generally been overlooked, however, that the nitrogen in dissociated ammonia might have an important effect on the sintering process and on the properties of stainless steel compacts. Considered an inert gas in many applications, nitrogen, on the other hand, is very reactive with cer- tain metals. Dissociated ammonia could not be used for hydriding zirconium or titanium. Nitrogen reacts with columbium, tantalum, chromium, uranium, thorium, and many other active metals. Iron and iron-base alloys are, for the most part, inert in nitrogen but there are many borderline cases. It has been reported that stainless steel stabilized with columbium or titanium should not be sintered in dissociated ammonia.3 olybdenum has been reported as reacting with dissociated ammonia to a minor extent.' Although most of the reactions with iron-base alloys are attributed to the action of un-dissociated ammonia and the action of nascent nitrogen, Uhlig4 showed how readily pure molecular nitrogen reacts with and diffuses into 18-8 stainless steel at 1150°C. He also pointed out how readily nitrogen diffuses out of 18-8 stainless steel when heated in pure dry hydrogen, and these thorough investigations on the subject show that commercial stainless steels are nitrogen-bearing, since they are melted in air. The effects of nitrogen in stainless steel, particularly the 18-8 Cr-Ni type, previously have received considerable attention." In 1926, it was pointed out

Jan 1, 1956

By Allen F. Agnew

Detailed stratigraphic studies in the Wisconsin-Illinois-Iowa district have made it possible to map the folds and faults that controlled the deposition of the zinc-lead ore. Prospecting on the basis of this mapping and prospecting in lower zones that are potentially ore-bearing have led to discoveries of ore. GEOLOGIC studies for the Federal and State governments in the Wisconsin-Illinois-Iowa zinc-lead district were begun in 1835, and subsequent surveys were made in the three states at intervals until 1916, see Table I. The current study of the district, Fig. 1, by the U. S. Geological Survey was begun in 1942 in the hope that a systematic investigation would help increase production of zinc and lead, then in extremely short supply. Major emphasis of the USGS program was on detailed mapping of the geologic structure and ore deposits. Preliminary maps and reports covering localities of intensive mining activity have been published during the course of this study, Fig. 2. By 1950 the objectives of the study by the USGS were revised; 71/2-min quadrangles of relatively unprospected localities as well as intensively mined localities are now being mapped in Wisconsin. Since 1945 the investigation in Wisconsin has been made in cooperation with the Wisconsin Geological and Natural History Survey, and since 1951 the geologic mapping of areas of particular interest in Iowa has been performed in cooperation with the Iowa Geological Survey. At intervals since 1943 the Illinois State Geological Survey has mapped the geologic structure and ore deposits of localities in the Illinois part of the mining district, see Fig. 2. Geology was applied by mining company personnel as early as 1853, but only sporadically, with periods of greater application between 1890 and 1925. Much of the so-called geologic work was in reality mining engineering. Since 1946 the major mining companies in the district have employed geologists who have successfully applied geologic techniques in the search for ore. History of Mining Occurrence of galena in the district was known as early as 1658 or 1659, when French explorers heard of lead mines that were apparently in the vicinity of Dubuque, Iowa. In 1690 a trading post was established near Dubuque to obtain galena. The first significant attempt at mining by white men took place in 1788 when the Indians granted to Julien Dubuque mining rights for 20 miles along the west side of the Mississippi River, including the vicinity of Dubuque, Iowa. By 1805 lead was being mined near Galena, Ill. In 1819 permanent settlement of the region was begun, and most of the important lead-producing areas had been found by 1830, see Fig. 3. Lead production in the Wisconsin-Illinois-Iowa district between 1830 and 1871 far exceeded that of any other district in the U. S.' Smithsonite was first mined in 1859, and sphalerite was mined as early as 1867. After 1873 the production of sphalerite exceeded that of smithsonite. In 1873 annual zinc production from the district first equaled lead production, and from then until 1893 production of zinc and lead was roughly the same. Since 1893 the ratio of zinc to lead mined has generally ranged between 5:l and 20:l. In 1942 the Wisconsin-Illinois-Iowa zinc-lead district ranked 14th among zinc-producing districts of the U. S. From 1946 until February 1953 the dis-

Jan 1, 1956

By E. C. W. Perryman

The recovery and recrystallization characteristics of superpurity aluminum have been investigated using electrical resistivity, X-ray line breadth, and hardness measurements for the former and the micrographic method for the latter. The three different properties recover at different rates and have different activation energies. The recrystallization results agree well with Avrami&apos;s theory and furthermore indicate that the perfect subgrains formed during recovery are not the nuclei for re-crystallization. WHEN a metal is plastically deformed, its physical and mechanical properties generally undergo considerable changes and by subsequent annealing these changes are partly or wholly annihilated. Thus, a recovery process can be discussed, taking this term in its general sense. In practice, however, there is reason to discriminate between two apparently different processes, one most easily followed at low temperatures, in which the properties return to an almost constant value between that of the cold worked and fully annealed material, and a second process in which the properties return to their original values before cold working and which is accompanied by the formation and growth of new grains having an orientation different from that of the matrix. In this paper the word recovery will be taken to mean the changes in some property as a function of annealing time which occur either without the appearance of new grains or under conditions such that the new re-crystallized grains are very small (= 2 microns), are very few in number, and substantially do not affect the property being measured. This definition is rather abitrary, for it will depend upon the sensitivity of the technique used for the observation of new recrystallized grains, which in the present work was about 1 to 2 microns. However, it is helpful to use the term recovery in this sense and to reserve the term recrystallization for the processes of nucle-ation and growth of new grains in the cold worked matrix. Although considerable work has been done on recovery and recrystallization, most workers have based their study on the measurement of one or perhaps two parameters. Since very small amounts of impurities have such a profound effect on the recrystallization characteristics of a pure metal, it becomes extremely difficult to correlate one piece of work with another. With this in mind, the present work on recovery and recrystallization was done on the same material. Experimental Procedure Material Used and Fabrication: The composition of the superpurity aluminum used throughout this investigation was 0.002 pct Cu, 0.003 pct Fe, 0.003 pct Si, and <0.001 pct Mg. The ingot was hot rolled to 0.250 in., annealed, and cold rolled to 0.034 in. A large number of reductions and intermediate anneals were carried out so as to produce material with a minimum of preferred orientation and maximum homogeneity. For the recovery part of the investigation, the final cold reduction was 20 and 80 pct and for the recrystallization part, 20 pct. After each pass in the cold rolling process, the material was quenched in cold water in order to keep the rolling temperature as near room temperature as possible. Annealing Procedure: For the recrystallization work, specimens 1x1 in. were cut from the 0.034 in. cold rolled sheet and a hole was drilled in each through which a wire was threaded to support it in the salt bath. The temperature of the salt bath was controlled to +2°C and the time taken for a specimen to reach temperature was approximately 5 sec. These 1 in. squares were then divided into three groups, one of which was given 5 min at 318°C and another 2 hr at 244°C. These treatments were such that recovery was almost complete and a well defined subgrain structure produced. Separate specimens of each group were annealed for different times at 301°, 318°, 355°, and 373°C, i.e., three specimens for each annealing time. The delay between finish of cold working and start of annealing was about 1 hr. For the recovery work, strips 0.062 in. thick were cut from the cold worked sheet, annealed, and then given the last cold rolling operation. This was done for each annealing temperature. By this means it was possible to minimize the delay between cold working and annealing. In general, all measurements were carried out within 1 hr of the last cold rolling operation. Annealing at low temperatures was done in an oil bath the temperature of which was maintained constant to +1°C. Electrical Resistivity Measurements: Strips 20x0.5x0.05 in. were machined and the electrical resistance measured using a Kelvin double bridge. Measurements were made in an oil bath maintained at 20rt0.1°C. The same specimen was used for the complete isothermal annealing curve.

Jan 1, 1956

THE strike and dip of bedded formations is readily determined by trigonometry if some marker horizon is intercepted by three holes. If no marker can be identified and if orientation of the cores is unknown, as is the usual case in diamond drilling, the determination still can be made readily by the use of a stereonet if the bearing, inclination, and angle the bedding makes with the core axis is known for each of the three holes. Such determination, valid only if the bedding orientation is fairly uniform within the area drilled, is considered simpler, faster, and more effective than any solution previously published. Method: The steps of this procedure are as follows: 1) Mark north and south poles on tracing paper placed over stereonet.* 2) Plot the three diamond drillholes by drawing a line from the center of the net in the direction of the bearings of the holes. Then rotate the paper until each line, in turn, lies along the equatorial diameter of the net; the end of each line is determined by the inclination of the hole measured in degrees from the periphery toward the center of the net along the equatorial diameter. Fig. 1 illustrates a vertical hole and a hole inclined at —23" due east. 3) With the projection of one diamond drillhole along the equatorial diameter, measure from the end of the hole, to the east and then to the west, a dis- tance in degrees equal to the core axis-bedding plane angle. Find two more points by measuring the same number of degrees north then south along the great circle from the end of the drillhole. Draw a circle, the center somewhere along the direction of the projection of the drillhole, to connect these four points. Draw circles for the other two diamond drillholes in the same manner. See Fig. 1 for two circles representing core axis-bedding plane angles of 35" and 23" and Fig. 2 for these plus a third circle representing a core axis-bedding angle of 42" in a hole bearing S 50 W inclined at —52". 4) Rotate the tracing paper until one great circle on the stereonet is found which is tangent to all three of the circles or parts of circles derived in the previous step. Trace this great circle on the paper and join its ends with a straight line passing through the center of the net. The bearing of this line is the strike of the bedding. In Fig. 2 the bedding strikes N 77 E. 5) Rotate the paper until the strike is along the polar diameter of the net. The dip of the bedding is determined by measuring along the equatorial diameter the distance in degrees from the periphery of the net to the great circle derived in step 4. The dip of plane illustrated in Fig. 2 is 55" to the N 13 W. Fig. 3 indicates the solution for three holes whose bearings and inclinations are N 20 W and —43o, due E and —30°, S 30 W and 23" with core axis-bedding angles of 30°, 50°, and 43" respectively. The bedding (stippled area) strikes N 44 W and dips 70" to the southwest.

Jan 1, 1956

By W. G. Pfann

Under certain conditions, a molten zone can be made to move through a solid by impressing a stationary temperature gradient across the solid. This phenomenon can be utilized in fabricating semiconductive devices, growing single crystals, joining, boring fine holes in solids, measuring diffusivities in liquids, small scale alloying, and purification. Fundamentals and exemplary applications are outlined. ANEW aspect of the travel of a molten zone through a solid is considered in this paper. Whereas, in previously described zone melting techniques,&apos;-&apos; zones were usually caused to move by changing the position or temperature of a heat source, in the present technique a zone is made to move by impressing a temperature gradient across it. For example, a thin layer of molten A1-Si alloy, sandwiched between two silicon slabs having a temperature gradient normal to the layer, will travel through the hotter slab. One feature of temperature gradient zone melting, as this technique will be called here, is that zones of unusually small dimensions can be maintained. This leads to such diverse uses as have been listed in the abstract. In this paper fundamentals of the movement of a molten zone in a temperature gradient, and some practical applications thereof, are outlined. Assumptions The movement of a molten zone through a solid body of solvent substance in which a temperature gradient exists will be discussed. The length of the zone will be its dimension in the direction of motion. The direction of the temperature gradient will be toward the region of higher temperature. To be considered is a binary or higher order solute-solvent system in which the concentration of solute in the molten zone is sufficient to produce a lowering of the freezing temperature of the solvent which is at least of the order of the temperature range impressed on the charge. While we discuss primarily molten zones in a solid matrix, the principles are applicable to solid or vaporous zones in a solid matrix, a requirement being that the diffusivity in the zone be substantially greater than in the matrix. Diffusion of solute into the surrounding solid will be assumed negligible. In general, its presence will not basically alter the conclusions to be drawn. For illustration, a system represented by the partial constitutional diagram of Fig. la will be discussed, in which k, the distribution coefficient defined in the figure, is constant and less than unity. However, the technique is applicable to any solute- solvent system in which one component lowers the melting point of another component. Movement of a Molten Zone in a Temperature Gradient Consider, in the system AB of Fig. 1, where B is designated the solute and A the solvent, the effect of sandwiching a thin layer of solid B between blocks of solid A and placing the whole in a temperature gradient such that the temperature of the layer is above the lowest melting temperature of the system. Surrounded by an excess of A, the layer will dissolve A, becoming molten, and expand in length." As so- lution of A continues, at both interfaces, the mean solute concentration in the zone will move to the right in Fig. la, until at temperature T, the liquid at the cooler interface reaches the liquidus concentration C,. Solution of A thereupon ceases because the liquid T1 is saturated with A. The liquid at the hotter end of the zone, being at temperature T2, is not saturated with A at concentration C1. Hence solution of A continues there and concentration C2 is approached. A concentration gradient therefore is set up in the zone, causing A to diffuse toward the cool end and B toward the hot end. As a result, the liquid at the cool interface becomes supersaturated and a layer of crystalline A containing concentration kc, of B in solid solution freezes. Since a source of A

Jan 1, 1956

By R. F. Krueger, L. C. Vogel

A design is presented for an electrical analog computer which can solve non-steady state heat transfer problems in an extensive radial forrnation containing a moving cylindrical source. The computer is used to simulate a .simplified thermal oil recovery process in which heat transfer from a moving, constant temperature source takes place radially by conduction only. Temperature distribution curves are .shown for several different assumed modes of travel for the heat source. The data are used to estimate the residual fuel requirements necessary to maintain a self-propagating isotherma1 front for the particular system being studied. Although the computer is designed to represent an unique system. conversion factors can he adjusted to show the effects of changing the assumed values of system constants, such as thermal conductivity of the formation and temperature of the source isotherm. Examples are given to illustrate the relative influence the assumed values of these variab1es will have upon the quantity of fuel required to maintain the source. The maximum effect of heat transfer by the flowing air stream is estimated mathematically, and full requirements for this system are shown to he markedly reduced. Inasmuch as the examples discussrd refer to a simplified process, the results are not directly applicable to a practical field operation. It is believed, however, that the data il1ustr-ate some general trends which are important in thermal recovery processes. Data from laboratory and field experimentation can he used to modify the computer to take into account the influence of heat transfer by various mechanisms, for example, by injected air and by fluids ahead of the hot zone. With .such refinements it would be possible to estimate more accurately the limiting values for the rate of travel of the high temperature front and for the required air- injection rates. Use of this computer should aid in evaluating the economic feasibility of oil recovery by various thermal processes. It is hoped this paper will stimulate further work by others to help accomplish this objective. As the costs of exploration for and development of new oil fields rise. increasing the recovery of oil from established fields becomes more and more important. In fields containing low gravity crude oil, ultimate recoveries by primary means are sometimes less than 10 per cent and often total only 10 to 20 per cent of the oil in place. Conventional secondary recovery methods are not always effective in increasing this total. Methods which have been proposed for increasing the recovery of viscous oils include thermal processes for increasing the mobility of the oil. One method is to provide a moving heat source generated within the formation to heat the oil and a flowing gaseous medium (for example, air) to sweep the oil to the producing wells. The possibility of such a process has intrigued engineers for many years.&apos;. &apos;." but little or no information has been available in the literature relative to the technical or economic feasibility of this method. Recently, however, interest has been revived by publication of laboratory and field test results indicating the feasibility of maintaining

Jan 1, 1956

By A. J. Teplitz, J. K. Rodgers, E. M. Pohoriles

This note is presented in order to call attention to a newly developed laboratory apparatus that appears to have interesting possibilities for the study of lost circulation of the pressure-parting type, for a more realistic evaluation of sealing materials for this type of loss, and for investigation of other aspects of hydraulic fracturing. A study of lost circulation, conducted jointly by operating divisions of the Gulf Oil Corp. and the Gulf Research & Development Co., has been in progress for the past few years. Earlier phases of the study dealt with mechanical factors contributing to loss of returns in laminar type sediments.&apos; One aspect of this type of loss which has been widely discussed in the literature and elsewhere concerns the geometry of the fractures into which such losses occur. This subject is not merely a philosophical one, but has an important bearing on procedures for combating lost circulation difficulties and on other well operations. The further course of the collaborative studies previously mentioned has produced some information on this subject which, though limited in amount, is believed to be significant. In several typical cases of lost circulation in laminated shale and sand formations, the wells have been surveyed with instruments2,3 capable of detecting the points of loss with considerable accuracy. These wells were located in the Gulf Coast of Texas and Louisiana, in the Texas Panhandle, and in the Rocky Mountain area. In each of these instances the loss was shown to be occurring at some distance removed from the bottom of the hole and sharply confined to a very narrow interval, less than 1 ft in thickness. It is rather difficult to imagine that fractures of a vertical nature&apos; would be of the limited extent indicated by the surveys in these wells. Furthermore, the high rates of loss at relatively low pressure differentials observed in some of these instances together with the narrow intervals involved would appear to require the radial flow pattern which would be associated with a more or less horizontal fracture plane. In view of the foregoing observations and records of successful squeeze cementing operations, in attempting to construct a laboratory apparatus For simulating pressure induced lost circulation, it was decided that the design should be based on a horizontal type of fracture. It was realized that5,6 Vhe production of horizontal fractures in a formation with non-penetrating fluid requires some mechanism for transmitting vertical components of the hydraulic forces to the plane of parting. This was accomplished, as will be evident in the description of the apparatus that follows, by providing recesses in the wall of the borehole which are believed to be representative of wellbore configuration found in Gulf Coast wells. The possible influence of such borehole irregularities on both pressure fracturing and the treatment of lost circulation appears to have been neglected in many studies of these subjects. It is believed that the present apparatus, incorporating features that take into account some of the factors mentioned, will provide means of gaining a further understanding of pressure induced fracturing and possibly for more realistically evaluating the numerous sealing agents, particularly the non-time-setting materials employed in treating the pressure-parting type of loss. DESCRIPTION OF APPARATUS The test cell used in the laboratory investigations is shown in Fig. 1. A schematic diagram of the entire system is shown in Fig. 2.

Jan 1, 1956

Jan 1, 1956

By E. W. Cawthorne, R. I. Jaffee, C. M. Craighead

SOLUTION of a solid metal or alloy in a molten metal bath is used daily in melting operations, extractive metallurgical processes, and in brazing. It is generally recognized that temperature, time, agitation, and the composition of the solute metal and the solvent bath all affect solution rate. However, there is little information available in the literature on the kinetics of the process or the relative effect that these variables have on solution rate. In connection with an aluminum brazing study, data on the solution of aluminum in an A1-Si* bath to promote rapid solidification. The chemical analyses were made on drillings taken from the cast plates. The results of this work are listed in Table I. The thermal-analysis data were obtained on 200 gram samples cooled at approximately 1.5" per min. A calibrated chromel-alumel couple was used. The thermal arrests were recorded autographically on a General Electric photoelectric potentiometer recorder. The instrument was calibrated to 22.5 pct. The thermal emf was bucked with a Leeds and Northrup semiprecision potentiometer so that 1 mv represented the full scale of the GE recorder. Referring to Table I, it will be noted that the analytical results tend to be lower than the intended compositions by about 0.3 pct Si in the higher ranges. In view of the known difficulties in obtaining accurate silicon determinations by wet analysis when the silicon content is high and in view of the care that was employed in weighing and preparing the alloys, the intended compositions are believed to be more accurate than the analyses. Furthermore, when the thermal-arrest data are plotted against the intended compositions, a smooth curve is obtained, as shown in Fig. 1. This is not the case when the data are plotted against the analytical results. It will be noted from Table I that the 12.5 pct Si alloy (melt 4) showed a primary arrest at 577.6"C and the eutectic at 576.l°C. The metallographic examination of this chill-cast plate sample showed a small amount of primary silicon. These results, Fig. 1, place the eutectic at slightly less than 12.5 pct Si and are in rather good agreement with the unpublished Hanford data. In all of the subsequent work, the composition of the A1-Si dipping baths was determined by thermal analysis (spread between the primary arrest and the eutectic temperature) employing 12.5 pct Si and 577.2 °C as the composition and temperature of the eutectic. Material Preparation and Selection of the Techniques: At the beginning of this work, it was anticipated that, owing to oxide film present on the surface of the aluminum, difficulty would be encountered in obtaining rapid uniform wetting of aluminum specimens dipped in the A1-Si bath. The following etchants were investigated as possible methods of providing a thin uniform oxide film on the specimen surface: 1—phosphoric acid (H³O4), 2—fluoboric acid (HBFI), 3—sodium hydroxide (NaOH), and 4—hydrofluoric acid (HF). Tests with sheet .specimens (2x½x0.06 in.) of 2s aluminum prepared with these etchants indicated that the fast uniform wetting required for this work could not be obtained if any oxide film existed on the specimen surface. Tests were then conducted by dipping similar specimens etched in 5 pct NaOH and given a thin

Jan 1, 1956

By A. Styka, G. Fischer, S. Tour

Described herein are the results obtained during research work involving coating titanium alloys with molybdenum by vapor-deposition methods. Results show that the method can be used successfully to deposit hard adherent wear-resistant coating of methodmetallic molybdenum on titanium or titanium alloys without changing the microstructure of the titanium base. PRODUCTION and use of titanium and its alloys have increased tremendously in the past few years. The physical, mechanical, and chemical properties of this engineering metal have caused considerable enthusiasm among metallurgists and engineers. However, as with all materials, there are some drawbacks. For example, titanium is susceptible to seizing and galling on wearing surfaces. In order to produce a good wear-resistant surface, many investigations have been conducted evaluating oxidizing, carburizing, nitriding, carbonitriding, sili-conizing, and chromizing of titanium. All of these processes require high temperatures for rather extensive periods of time. It has been possible to produce hard surfaces on titanium and its alloys by a number of these processes at the expense of a deterioration of the physical properties of the base material. A practical solution to the problem of providing titanium and titanium alloy parts with a satisfactory wear-resistant nongalling surface must be one that does not involve excessive temperatures for long periods of time. Sam Tour & Co. Inc. has completed a research and development contract for the United States Army Ordnance Corps on vapor deposition of molybdenum on titanium and titanium alloys. On the basis of results obtained from the research program, titanium alloys can be coated successfully with molybdenum to provide a hard wear-resistant surface without harm to their base mechanical properties. The remainder of this article is a description of the techniques used to apply the coating and the results obtained from wear tests on molybdenum-coated titanium. Theory Basically, the technique used was the application of molybdenum by a vapor-deposition method, thermal decomposition of molybdenum hexacarbonyl [Mo(CO)] with hydrogen as the carrier gas. The selection of this method was based chiefly on the following considerations: 1—low plating temperature which would minimize excessive grain growth, 2— low decomposition temperature of the carbonyl, 3— possibilities of controlling the hardness of the plate by adjusting the carbon content using the plating temperature and pressure as the primary variables, 4—use of high vacuum, thereby avoiding unnecessary oxidation and other complex reactions with the atmosphere. Free energy data1 show the strong tendency for titanium to combine with O2 N2 or carbon from normal temperatures to temperatures above its melting point. To maintain the titanium in a film free condition, the use of as high a vacuum as possible is indicated. The literature&apos; indicates that the reaction product of hydrogen with titanium is unstable in vacuum at around 400°C. 5—Although it is indicated from the thermodynamic standpoint that there is little possibility of removing carbon from either titanium or molybdenum, the work of Lander and Germer -ndicates that the use of a suitable H,/CO ratio is somewhat effective in minimizing carbon deposition. 6—Availability of molybdenum carbonyl. In the simplest form, the conditions of equilibrium3 in chemical reactions involving decomposition of carbonyl are as follows: Mo (CO) ? Mo + 6CO 2CO * C + CO,. The plating rate is proportional to the rate of evolution of CO from the decomposed carbonyl, i.e., it is proportional to the pressure of the gaseous decomposition products. Carbon released from CO gas is the significant constituent for the variability of the physical properties of the product. High carbon deposition is favored by increasing pressure. Limitations are imposed in the selection of plating temperature and pressure. Excessive temperature re-

Jan 1, 1956

By Louis A. Panek

MOST roof bolts are used in mines with bedded roofs, but it has not been determined to what degree thin-bedded roofs can be reinforced by bolting if there is no thick member in which to anchor the bolts, or what function the bolts must perform in such a case. Owing to widespread practice of sys- tematic bolting to support thin-bedded roofs, moreover, it is desirable to design roof-bolting systems on a quantitative basis. Specifically, a solution to the following problem is required: For a roof composed of beds of given thickness and physical properties, what is the optimum length, spacing, orientation, and tightness of bolts consistent with safety and economy? The investigation reviewed here has produced a functional equation to evaluate these variables and establish basic principles of roof bolting.

Jan 1, 1956

By R. E. Hurst, D. E. Ramsey, J. M. Moore

The "frac" method of well stimulation has been applied successfully to all producing formations in the Permian Basin area. During the five years since its development, many changes and improvements have been made in treating materials. procedures, and equipie11t. A number of fluid carrying agents, having different physica1 and chemical properties, have been developed to meet variorus well requirements. The current trend is toward larger gallonage treatments, employing higher injection rates. The use of "down-the-casing" techniques has greatly reduced high surface working pressures, attributable to friction losses resulting from injection throrugh tubing. Petrographic studies of various Permian Basin formations, coordinated with laboratory and well log data, have been found a valuable guide in planning frac treat111o1t.s. A knowledge of the extent (and orientation of naturally occurring fractures and planes of weakness in the formation, aid in predicting the ultimate drainage pattern resulting from the frac treatment. INTRODUCTION The South Permian Basin covers an area in Wcst Texas and New Mexico about onc-half the size of the state of Texas, This vast region has been called the "Permian Basin" for so long that the term will he used here. It includes an area south of the Matador Arch. approximately 250 miles wide and 300 miles long. Structural features of importance within the basin are the Northwest Shelf, Eastern Platform, Midland Basin, Central Basin Platform, and Delaware Basin. The principal producing formations include sand, limestone and dolo-mite, with lesser amounts of shale, anhydrite. chert. and various silicates. All of the producing formations in the Permian Basin have responded to some type of frac treatment. Essentially, a frac treatment may be defined as the injection, into a formation. of a fluid carrying agent containing a particulated solid (usually sand), for the purpose of increasing production. The application of this method of well stimulation to many differing Permian Basin reservoirs has necessitated numerous changes and improvements in carrying agents, solids, service equipment. well equipment. and treating techniques. CARRYING AGENTS A number of different types of fluid carrying agents have been developed since the introduction of the frac method of well stimulation. These agents have different physical and chemical properties, and in many cases the extent of production increase derived from the frac treatment depends on the choice of fluid carrier. Unfortunately, due to many different systems of nomenclature used in the oil field, these differences are not always recognized by the oil Operator. In general, carving agents may he divided into the following broad classi-

Jan 1, 1956

By L. A. Rapoport

This paper is intended as an aid in the perfornzance and interpretation of experimental studies of multi-phase flow in porous tnedia. The mathenmatical formulation of incompressible, two-phase flow phenomena in a three-dimensional porous medium is presented. The resulting equations which account for the effects of gravitational and capillary forces are used to derive general scaling laws permitting accurate representation of water-oil displacement processes by means of experimental flow models. The significance of the scaling laws is examined in the light of the physical concepts of micro-behavior of fluids in porous media. Formulations of scaling con(litions obtained by application of dimensional analysis are reviewed. The principles of application and the limitations of flow model studies are discussed. INTRODUCTION Most of the problems facing a reservoir engineer involve three-dimensional, two-phase flow systems. influenced by the effects of gravitational and capillary forces. Present computational procedures generally do not permit the evaluation of such systems without introducing greatly simplifying assumptions. The actual reservoir configuration is usually replaced by one or a combination of several "equivalent" linear systems, and the effects of capillarity and gravity are considered to be negligible. While these assumptions may in many instances be justified, there are a number of important practical problems for which the results obtained on the basis of such simplifications remain open to question. An alternate approach to the problems that are not amenable to analytical treatment consists of seeking their solution by experimental laboratory investigations. The main difficulty of such investigations lies in the fact that multiphase flow phenomena subjected to gravity and capillary forces proceed differently at different rates and in systems of different dimensions. Therefore, unless great discrimination is exercised in selecting the conditions and interpreting the results of laboratory tests, such tests may be entirely misleading in regard to field applications. The purpose of this paper is to present a theoretical background for the performance of laboratory tests that are more nearly representative of field behavior. It will be shown that simulation of field behavior can be achieved by conducting laboratory tests under conditions selected in accordance with definite scaling laws. The formulation of conditions required for the scaling of two-phase flow experiments in porous media has been presented in the literature on several occasions.12,3,4 One of these formulations advanced by Leverett1, cannot be considered applicable to most practical cases inasmuch as it does not cover generally the regime of laminar flow. An adequate treatment, based on the consideration of dimensional analysis, was presented by Engelberts and Klinkenberg.2 Their treatment, however, is concerned primarily with the scaling of linear flow systems, and hence somewhat limited in scope. Accordingly, the formulation of more general scaling laws, applicable to three-dimensional systems, appeared to be warranted. It appeared, furthermore. desirable to establish this formulation on the basis of a mathematical treatment, rather than by application of general principles of dimensional analysis, to permit more explicit

Jan 1, 1956

By Frank G. Miller, Ralph A. Seban

Problems relating to thermal methods of oil recovery have been given increasing attention during the past year. The nature of the physical and chemical processes underlying thermal recovery are not yet well understood. The need for pertinent basic information is recognized generally. One of the processes involved is the transfer of heat by conduction in oil reservoir rocks containing moving reservoir fluids. This technical note deals with heat conduction in a laboratory sand column filled with a moving hydrocarbon and therefore should be contributory to the presently inadequate fund of knowledge on thc over-all subject. In an analysis of the flow of vaporiziny propane through a horizontal column of sand, one of the present author9 demonstrated correspondence between thc measured values of pressure along the length of the column and those predicted by a theory which postulated that the enthalpy of the propane was invariable along the length of the column. This postulate way implied as a deduction from the principle of conservation of energy but the details of the deduction were not given. The specific purpose of this technical note is the presentation of these details both as an adjunct to the earlier analysis and to supply some additional details on the processes involved in this type of flow. Results disclose that rates of heat transfer by conduction, in the direction of fluid motion, generally would be small for systems of the type studied. FUNDARIENrAI. ENERGY EiQUAI-[ON The principle of conservation of energy may be applied to a section of the porous material on the basis that heat transfer, like fluid flow, is possible in the x direction only. Transfer of heat in the y and z di&apos;rections is prevented by suitable insulation or by taking the medium as infinite in directions perpendicular to the x axis. For steady state heat conduction and conditions of steady fluid flow the principle of conservation of energy specifies that any reduction in the enthalpy rate increases the flow of heat in the same proportion. Stated mathematically, dH KA 87 —- = - — - — U) * dx W dx........ Lvhere is the flow of heat in the positive x W dx direction. TEMPERATURE DISTRIBUTION IN DIRECTION OF FLOW The column of sand used in the previoi~sly described research is divisible into three different flow regimes. each of which may be analyzed independently. In the entrance region the liquid approaches the saturation state. A transition region is postulated following the transverse section at which the saturation state of the liquid is attained. In this transition region gas and liquid phases are both envisioned as present, with no vaporization occurring and with fluid movement restricted to the liquid. The upstream end of the exit region is at the transverse section of the column where the fraction of the pore space occupied by gas first becomes great enough for gas flow and where vaporization of the liquid begins. Fig. 1 indicates schematicaHy the thermodynamic processes undergone hv the fluid in the three flow regimes.

Jan 1, 1956

By C. S. Matthews, W. R. Strickler, M. Prats

To gain an insight into the deviations from normal behavior caused by dip. a mathematical study has been made of single-fluid five-spot floods in dipping reservoirs for flooding techniques likely to be employed in such cases. Streamline patterns and sweep eficiencies are computed for a number of different cases, and the results, where possible, are presented in graphical form. An increase in sweep efficiency can be obtained by moving the central injection well updip, and the opti~num position is found for several cases. The applicnhility of the results is discussed. INTRODUCTION Because of the growing importance of water flooding in California and in other locations where large angles of dip are quite common, it is important to know at least some of the effects of dip on the performance characteristics of water floods in such instances. In the past, only reservoirs having relatively mild dips have been wateflooded. Consequently, little is known today as to the effect of dip on the performance characteristics of a flooding operation from the point of view of field experience; and because of the complexity of the problem, little, if anything, has been done on the problem from the point of view of theory. There are two distinct aspects of the role played by gravity in a flooding operation. The first is that of the preferential segregation of the reservoir fluids at the time when the flood is to commence. The second is the role that it may play in affecting the performance of the reservoir during the course of the flooding operation. In this paper the reservoir is assumed to be filled with only one fluid, so that there is no preferential segregation of reservoir fluids at the commencement of the flood. Moreover, the injected and in-place fluids are assumed to have the same characteristics, so that in effect we consider only a single-fluid problem. Single-fluid results have been used as a guide in the past for predicting and interpreting the behavior of regular five-spot floods in horizontal reservoirs. It is thought that single-fluid results might likewise be used for five-spot patterns in dipping reservoirs as a norm to which the effects of the multifluid problems might he referred.* In confining our attention to the single-fluid case, we therefore do not consider the preferential segregation of injected water in the oil bank, or of the oil bank in the unflooded zone. Instead we consider the deviation from the behavior of a horizontal five-spot which is caused by use of flooding techniques (i.e., the flow potential pattern at injection and production wells) likely to be employed during flooding operations in dipping reservoirs. In other words, we consider effects which are caused by the pattern of injection and production well pressures which we choose to apply. Performance characteristics are given for the five-spot spacing pattern as a function of two parameters; one is the ratio of gravity head to potential difference bctwccn the high updip injection well and the low downdip producer of the same five-spot, denoted by Rg; the second is the orientation of the five-spot pat-

Jan 1, 1956

By L. D. Jaffe

From the limited experimental data in the literature, preliminary values were derived for the thermal diffusivity of titanium alloys and for the quenching severity of various mediums used in heat treating them. The thermal diffusivity, under quenching conditions, was found to be approximately 0.006 sq in. per sec. The quenching severity H for brine is approximately 8, for water 4, for oil 0.9, for air 0.08, and for argon 0.02 in. -&apos; The quenching severity of the Jominy-Boegehold end quench water jet against titanium alloys appeared effectively infinite. Using these results, graphs were prepared showing ideal round sizes and Jominy positions having cooled conditions equivalent to those at the center and surface of titanium alloy rounds, plates, and sheets quenched in various media. THE importance of proper quenching of steel parts has long been recognized, and much quantitative work has been done on the subject. Recently, it has become evident that for titanium alloys, too, the rate of cooling from high temperature is important in obtaining high strength and hardness. Maximum hardness and strength may not be attained in the as-quenched condition but rather after a subsequent tempering or aging treatment. Nevertheless, if cooling from temperatures near the ß transus is too slow, for the hardenability of the alloy used, a soft a-ß structure will be produced which will not harden on subsequent aging.&apos;-" The quenching of parts of practical interest can usually be approximated by simple shapes, such as cylinders (rounds) and plates (or sheets) of various thickness and combinations of these. A standard that has been used extensively for comparison purposes is the center of an ideal round: a cylinder quenched in a medium that instantly cools its surface to room temperature." For steel, considerable practical use has been made of the Jominy-Boegehold end quench hardenability specimen,".&apos; and its value for titanium alloys is becoming evident. It therefore appeared worthwhile to attempt comparison of cooling conditions in titanium alloy rounds and plates of various sizes quenched in various media with cooling conditions in ideal round and Jominy quenches. These comparisons are based upon measurements reported in the literature. Quenching Severity of Jominy Water Jet and of Brine As one starting point, there were available the data of Phillips and Tobin8 for positions on a Jominy specimen having the same hardness as the centers of round bars of various size quenched in 5 pct NaOH brine, shown in Table I. The Jominy speci- men is a round bar, normally 1 in. diam and 4 in. long, quenched by a water jet at one end and air cooled on the other surfaces.&apos; After quenching, hardness is measured vs distance from the quenched end on longitudinal flats ground 0.015 to 0.10 in. deep. The data of Table I were based on a subsized specimen of 3/4 in. diam. Since the positions tested are close to the jet quenched end, cooling there may be taken as due solely to the jet, and air cooling can be neglected. These positions are then equivalent to various locations near one surface of an 8 in. plate jet quenched on both sides. Assuming that the thermal diffusivity is constant and that Newton&apos;s law of cooling holds, temperature vs time curves at corresponding positions in Jominy specimen and round bar then may be calculated for various assumed quenching severities of the water jet and of the brine. Cooling curves are generally taken to be metallurgically equivalent when they show the same time to reach a temperature halfway between the initial (heat treating) temperature and the final (quenching medium) temperature.5 On this basis, using Russell&apos;s tables,9 upplemented by heat flow tables derived in similar fashion by the author for positions near the surface of severely quenched plates, it was found that the experimentally observed equivalence, Table I, was best matched if the quenching severity H of the Jominy water jet was taken as infinite (H = co). This means that the jet quenched surface should be considered as instantly cooled to the temperature of the water

Jan 1, 1956

By W. F. Stowasser

downdraft traveling grate process to agglomerate pelletized iron ore concentrates has been successfully demonstrated in a pilot plant at Carrollville, Wis. Work there followed several years of development in the Allis-Chalmers Mfg. Co. laboratories, and the pilot plant phase was carried out in cooperation with Arthur G. McKee & Co., consultants and engineers to the iron and steel industry. End result of the process is conversion of iron ore concentrates into a form which can easily be transported and smelted in the blast furnace. Process Description The first of two process steps incorporates the art of balling and prepares the concentrates for burning. The second step consists of burning the green balls on the grate machine to the hardness required for shipping and handling purposes and for reduction in blast furnaces, see Fig. 1. Facilities are provided at the pilot plant to receive carload quantities of concentrate. The concentrates are loaded into a 50-ton bin direct from railroad cars. Because of the variable moisture content of the concentrates after shipment in an open railroad car it is necessary to repulp and refilter the concentrates to maintain a uniform and proper moisture content for the balling operation. Concentrates are conveyed to slurry tanks, and the slurry, at 50 to 60 pct solids, is pumped to a 4x4-ft drum filter. The filter provides feed of uniform moisture to the plant. Magnetite concentrates are normally filtered to produce a cake containing about 10 pct moisture, a necessary requirement for the following balling operation. The filtered concentrate is conveyed to a rotary bin table feeder which acts as a surge bin for the filter cake and delivers a steady flow of concentrates to the balling drum. It is often desirable to make additions to the concentrates as they are fed to the balling drum. These additives, such as bentonite, increase the strength of the finished green pellet and improve ballability of the concentrate. A vibrating feeder supplies additive to the feed belt, and the additive is mixed with the concentrate in the balling drum. The balling drum, shown in Fig. 3, is 8x3-ft diam. An oscillating cutting bar maintains the lining in the drum by trimming off the buildup of excess concentrate as it forms. The drum is operated in closed circuit with a lx4-ft rod-deck vibrating screen. Undersize pellets or seed pellets from the screen are returned to the balling drum until they grow to the desired size. Size of pellets is controlled by the opening in the screen deck. The formation of pellets in the balling drum is affected by many variables. Some of these are: the size distribution of the feed, the particle shape of the concentrate, the feed rate to the drum, the moisture in the concentrate, the speed of rotation of the drum, the slope of the drum, and the type of trimming obtained with the cutting bar. In this process, attempts are made to control the pellet size within the limits of % to 5/8 in. diam. The screened oversize pellets are conveyed under a coal feeder where sufficient powdered coal is added to the belt to produce desired results in the burning process. The top size of the coal successfully used has been 20 mesh, and anthracite was used in the test program. Fig. 4 illustrates the vibrating screen and the coal feeder. The pellets and free coal are conveyed together to the 5x3-ft diam- reroll drum that rolls the coal onto the surface of the pellets. This drum is also equipped with a cutting bar. The prepared pellets, containing bentonite, water, and surface coal, are elevated to the traveling grate, which consists of a continuous strand of 37 pallets. Each pallet, with a grate bar area 2 ft wide by 1 1/2 ft long, has 14-in. high side plates, Fig. 5. Feeding and distribution of the green balls to the grate is handled by a short conveyor which oscillates back and forth across the 2-ft width of the grate. An adjustable vertical plate located several inches in front of the head pulley of the oscillating conveyor controls the height of the bed and levels the moving bed of pellets. This method of feeding prevents segregation of various size pellets as well as fines and produces a uniform, permeable bed. The pallet train moves under the furnace and across four windboxes, located beneath the pallet frames, see Fig. 2. As the green pellets are deposited on the grate, partial drying of the pellets begins over a 2-ft long updraft windbox. The low temperature air reduces the moisture in the pellets in the lower level of the bed and this operation is essential to prevent sagging of the bed during later stages of the Process. The air used for this drying is recuperated from cooling the pellets on the grate, and supplemental heat, required for starting the Process, is obtained from an auxiliary burner. The pellets are then moved by the grate into the furnace and over an 8-ft windbox, designated as the downdraft waste windbox. Products of combustion are exhausted from this windbox to atmosphere. The furnace, shown in Fig. 6, is constructed with three chambers to provide downdraft drying, preheating, and ignition, respectively, to the pellet bed as it passes through. Overall length of the furnace is 5.57 ft; however, the exterior wall ends may be moved to reduce the length and also adjusted to Obtain the bed height desired, The drying, preheating, and ignition sections of the furnace are supplied with medium temperature

Jan 1, 1956

By E. W. Stewart, G. P. Conard, J. F. Libsch

The effects of several additives upon the reduction characteristics of hydrogen-reduced ferrous formate are described. The various additives inhibit sintering of the reduced iron particles by apparently different mechanisms. The magnetic properties of the low density compacts produced from the resulting ultra-fine iron powders were improved markedly. THE permanent magnetic characteristics of ultra-fine iron powder prepared by various means have been a subject of considerable interest and experimentation in the past few years. When such particles are small enough to show single domain behavior, they possess&apos; 1—permanent saturation magnetization, and 2—high coercive force. In the absence of domain boundaries, the only magnetization changes in a particle occur through spin rotation which is opposed by relatively large anisotropy forces. With decreasing particle size, the coercive force tends to increase to a maximum and then decrease because of the instability in magnetization associated with thermal fluctuations. Kittel&apos; has calculated the critical diameter at which a spherical particle of iron can no longer sustain domain boundaries or walls to be approximately 1.5x10-&apos; cm. Stoner and Wohlfarthr in England and Neel4,6 in France have shown from purely theoretical calculations that the high coercive force expected from single domain particles is dependent upon crystal anisotropy, shape anisotropy, or strain anisotropy contributions. Further work by Weil, Bertaut,&apos; and many others has contributed much to the understanding of fine particle theory. Neel and Meikeljohn" have demonstrated that a decrease in particle size below a critical value of approximately 160A leads to a quite rapid decrease in coercive force because of the prevention of stable magnetization by thermal agitation. Lih1, working with powders prepared by the reduction of formate and oxalate salts of iron, has shown the marked influence of powder purity upon magnetic properties. Maximum coercive force was obtained in powders of approximately 65 pct metallic iron content while the maximum energy product, (BxH) occurred in powders of 85 pct metallic iron content. Careful consideration of the preceding theoretical considerations and experimental results has led to the manufacture of permanent magnets from ultra-fine ferromagnetic powders by powder metallurgy techniques. Such work has been done by Dean and Davis," the Ugine Co. of France, and Kopelman." The aforementioned work of Kopelman and the Ugine Co. was concerned somewhat with the effect of various additives upon the properties of hydrogen-reduced ferrous formate. Virtually no work, however, has been published on the effects of additives on the reduction rates of metal formates, although unpublished work by Ananthanarayanan16 howed promise of improved energy product in ultra-fine iron compacts prepared by the hydrogen reduction of a coprecipitated mixture of magnesium and ferrous formate. After consideration of the preceding information, it was hoped that a better balance between the metallic iron content and particle size of the reduced iron powder could be accomplished by a prevention of the attendant sintering of the partially reduced iron powder during the reduction reaction. It appeared possible that magnesium oxide might interpose a mechanical barrier between adjacent iron particles and prevent their sintering together, while metallic cadmium and metallic tin would interpose a liquid barrier which might accomplish the same purpose. The degree to which these materials were effective in accomplishing the foregoing objective and the experimental details associated with the work are reported in the following sections of this paper. Experimental Procedure Preparation of Formate and Oxide Mixtures: To obtain ferrous formate of reproducible reduction characteristics, a slight modification&apos; was made in the technique of Fraioli and Rhoda." A supersaturated solution of ferrous formate was mixed with an equal volume of 95 pct ethyl alcohol and the formate crystals precipitated by stirring and screened to —325 mesh. These crystals were in the shape of elongated hexagons, approximately 4x10 micron in dimension. Various preparations of such ferrous formate, designated as lot 111, were reduced for 2 hr, yielding ultra-fine iron particles of exceedingly reproducible size, metallic iron content, and magnetic properties. The magnesium and cadmium formates were prepared by the reaction of dilute formic acid with their respective carbonates, while the tin formate was prepared by the reaction of dilute formic acid with stannous hydroxide. To evaluate the effect of metallic formate additives in intimate mixture with the ferrous formate, varying amounts of magnesium, cadmium, and tin formates were coprecipitated with the latter. The designations of these materials and their chemical compositions are given in Table I. Due to the differing solubilities of the various formates in aqueous media,

Jan 1, 1956

By R. L. Smith, I. G. Greenfield

The binary system Ga-Sb has been investigated by thermal, X-ray, and metallo-graphic methods. &apos;The intermetallic compound GaSb melts at 705.9OC and forms a eutectic with antimony at 11.8 atomic pct Ga. This eutectic melts at 589.8OC. A eutectic appears to be formed at 29.8°C but is too close to the composition of pure gallium to be detected. IN the course of an investigation of the semiconducting properties of the intermetallic compound, GaSb, the phase equilibrium between gallium and antimony has been investigated. Recently, the phase diagram of similar systems, such as In-Sb,&apos; In-AS,&apos; and Bi-As3 have been determined. These diagrams have the same general appearance in that an intermetallic compound is formed at 50 atomic pct and a eutectic is formed on both sides of the intermetallic compound. Jenny,& who has been investigating the semiconducting properties of intermetallic compounds, has concluded from thermal data of several alloys that the phase diagram of the Ga-Sb system resembles those mentioned previously. This paper represents a more detailed study of the Ga-Sb equilibrium. Experimental Procedure The gallium that was used to prepare the alloys was obtained from A. D. Mackay Inc. and the Aluminum Co. of America; the latter reported the purity as 99.95 pct. The antimony was obtained from Bradley Mining Corp. who specified a purity of 99.997 pct. Since the intermetallic compound of GaSb was prepared primarily to be used for further studies of the semiconducting properties, additional purification by a standard zone-melting technique under an atmosphere of hydrogen was performed. Hall-effect measurements on this material indicated an impurity content of less than 3 ppm.5 The antimony also was purified by zone melting and used in conjunction with the compound GaSb to make the necessary alloys for the determinations of the antimony-rich side of the phase diagram. The antimony-rich alloys were chill cast in Vycor tubes which were evacuated to a pressure of less than one micron. Since these alloys expand on freezing, precautions were taken to prevent oxidation of the ingot in the event the tube fractured. To insure homogeneity, the brittle alloys were ground and then placed in the furnace for the thermal-arrest determinations. Since the cost of gallium is high, the experimental procedure was complicated somewhat because of the necessarily limited sizes of the melts. In order to economize, the gallium-rich side of the diagram was determined by using a 35 g ingot of pure gallium initially and adding increasing amounts of antimony in order to obtain additional alloys. The furnace used in the determination of the cooling curves is illustrated in Fig. 1. A 2¼ in. quartz tube, sealed at one end, was fitted with a brass flange which was attached with DeKhotinsky cement. The brass collar was water cooled to prevent the cement from softening. An "0" ring was used to provide a seal between the brass collar and the furnace cover. Nichrome ribbon was wound around a 2 ½ in. asbestos-covered copper core which was used to reduce the thermal gradient in the furnace. The insulation consisted of alternate layers of asbestos and aluminum foil surrounded by sil-o-cel refractory and

Jan 1, 1956