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By Louis A. Panek

The practice of roof bolting or rock bolting to stabilize rock surrounding underground excavations has increased tremendously within a few years. This widespread application has led to many questions concerning the mechanics of bolting and has pointed up the need for a quantitative method of designing bolting systems. To answer these questions a research program was initiated to determine the principles of roof bolting. The first problem chosen for investigation was the use of bolts to reinforce bedded roof, since the great majority of bolts are used under these conditions. The attack employed is a combination of theoretical and experimental stress analysis. Centrifugal testing of models was chosen as the experimental method because it is particularly suited to the study of stratified roof. This report describes the models, the experimental method, and the model-prototype relations. By using dimensional analysis, a general expression for a roof-bolting design formula in terms of the structural variables has been obtained. Certain model-prototype similarity requirements have been relaxed, thereby minimizing the number of variables to be studied and extending the applicability of quantitative test data to a large class of full size structures.

Jan 1, 1956

By S. C. Sun

With the aid of emulsifiers, intense high-frequency sound waves are capable of emulsifying any collector in water. The data show also that ultrasonically emulsified collectors are more effective in floating minerals than the nonemulsified collectors. THE use of ultrasonics in forming emulsions is not new. As early as 1927 Wood and Loomis reported preparation of emulsions with ultrasonics. In 1935 Rschevkin and OstrawskyV escribed the use of great ultrasonic power in producing fine emulsions of various oils and paraffin in water. Recently Oyama and Tanaka3 employed ultra-emulsification to increase the effectiveness of sodium ethyl xanthate in flotation of chalcopyrite and galena. An emulsion is a two-phase system consisting of two incompletely miscible liquids, the one being dispersed as finite droplets In the other. The dispersed liquld is known as the internal or discontinuous phase, and the surrounding liquid is termed the external or continuous phase. There are two types of emulsions; one is oil-in-water (O/W) and the other water-in-oil (W/O). The word oil refers to the liquid other than water. Circumstances exist in which the emulsion type is not clearly defined, and the internal and external phases both contain portions of the opposite phase. This is said to be a dual emulsion. Among the many hypotheses, 5a, B proposed for the formation of emulsions, the Bancroft's adsorbed film or double interfacial tension theory is widely accepted. Bancroft 7, 8 deduced that in the process of emulsification the interfacial tension between oil and water is lowered by the formation of an emulsifying film, which contains the adsorbed molecules and/or ions from the emulsifying agent and the two liquids. This film has two interfacial tensions, one with the water and the other with the oil, which are not necessarily equal. The difference in interfacial tension between the two surfaces of the film is chiefly responsible for forming different types of emulsions. For example, if the interfacial tension between water and film is less than that between oil and film, the film will become convex on the water side, thereby tending to form an oil-in-water emulsion. On the other hand, if the interfacial tension between water and film is greater than that between oil and film, the film will become concave on the water side, thereby tending to make a water-in-oil emulsion. In line with this theory, emulsifying agents soluble in water have the tendency to form oil-in-water emulsions, while those soluble in oil form emulsions of the reverse type. Apparatus and Experimental Procedure: The ultrasonic apparatus shown in Fig. 1 consisted of a hypersonic generator (A), Brush Development Co. model Bu-204; a hypersonic transducer bowl (B) whose resonant frequency is 400 kc per sec; and a round-bottomed glass tube (C) of 2.2 cm ID and 21 cm in length. The acoustical output power of the hypersonic transducer bowl was standardized with a Hewlett Packard vacuum tube voltmeter, model 41 0B, across the hypersonic generator output. The glass tube, containing the materials to be emulsified, was placed 1 cm above the central surface of the transducer bowl, which was filled with water as shown in Fig. 2. Ultrasonic emulsification was performed in three steps, although a one-step method has been used: 1) emulsifying the predetermined amounts of col-

Jan 1, 1956

It has been established that molybdenum sesquisulphide, not molybdenite, is in equilibrium with molybdenum metal and sulphur vapor in the vicinity of 1100°C. The S2 pressure for this system has been obtained using the Knudsen orifice method and the standard free energy for the dissociation of S2. THIS work was undertaken to help in determining the thermodynamic properties of the molybdenum sulphide which is in equilibrium with metallic molybdenum and sulphur vapor in the temperature range 1025" to 1150°C. From the results of MontoroL and of Parravano and Malquori' molybdenite would be expected to be in equilibrium with molybdenum metal, while the results of Guichard indicate that a lower sulphide must be in equilibrium with the metal. Thus it was concluded that the problem warranted reconsideration, especially in view of the suspiciously low temperature independent term for the standard free-energy function for the reaction MoS² Mo + S,. The reaction was calculated and duly noted as being low by Richardson and Jeffes,' using the data of Parravano and Malquori.' Experimental Method The general method used in this investigation is that of the Knudsen orifice method for the determination of equilibrium pressure. The apparatus and technique are similar to those described for the determination of the vapor pressure of silver.% owever, a closed-end McDanel tube instead of fused silica was used to maintain the vacuum, a molybdenum effusion cell with a replaceable lid was employed instead of a silica cell, and a titanium getter maintained at run temperature was used to assure that no oxidation of the molybdenum or molybdenum sulphide was taking place. All runs were made at a residual pressure less than 10-5 mm Hg. The data are given in Table I. Runs 1 through 13 were obtained using molybdenite, analyzed 98.5 pct, from the Molybdenum Corp. of America. The remaining runs were done with a sample from the Climax Molybdenum Corp. which was their grade No. 3 and analyzed 59.87 pct Mo. The weight loss of the cell during heating up and cooling down was subtracted from the total weight loss of the cell during the run. Also, when the tem- perature was changed, the Knudsen cell was placed in the vacuum chamber and heated at temperature for several hours in order to allow the sulphide and the metal to adjust their compositions to the equilibrium values, to desorb or adsorb gases into or from the molybdenum cell itself, and to desorb any water from the molybdenum sulphide or molybdenum powder inside the cell. Water may have been adsorbed inside the cell because, after each run, the top of the cell was removed and the material in the cell was stirred to insure that a layer of molybdenum metal would not build up and obstruct the passage of sulphur vapor into the gas phase. It was established that the molybdenum cell alone decreased in weight an inappreciable amount when heated at the highest run temperature for long periods of time. There are two questions to be answered before the data in Table I can be used to calculate thermodynamic functions: 1—Which molybdenum sulphide is in equilibrium with molybdenum metal and sulphur vapor? 2—What sulphur species are present in the vapor phase? It can be assumed safely that no molybdenum is vaporized, since its vapor pressure is almost negligible at these temperatures. It will be shown subsequently that no sulphide of molybdenum is volatile. Question 1 was answered in the following way: The especially purified molybdenite, obtained from the suppliers mentioned previously, was charged

Jan 1, 1956

By C. B. Jordan

LAVES and Wallbaum' have described TiRu and TiOs as having the same structure as TiFe; they had previously described the latter compound as having the CsCl structure. On the other hand, a careful investigation of the structure of TiFe by Duwez and Taylor- ailed to reveal the ordered CsCl structure, finding instead a random arrangement of titanium and iron atoms on the points of a body-centered-cubic space lattice. Consequently, it is not clear whether Laves and Wallbaum proposed the ordered or the disordered structure for TiRu and TiOs. In order to settle this question as to the structural type and to obtain values of the lattice para- meters (thereby completely determining the structures), the present investigation was undertaken. Samples having the compositions TiRu and TiOs were weighed out accurately from iodide titanium supplied by the New Jersey Zinc Co., ruthenium powder from Goldsmith Brothers Smelting & Refining Co., and osmium powder from Wildberg Brothers Smelting & Refining Co. No analysis was made of any of these metals. According to the respective analyses of the suppliers, total impurities amount to less than 0.03 pct in the titanium and to less than 0.5 pct in the osmium. The purity of the ruthenium is not known. The alloys were prepared by arc melting in a furnace of the type described by Schramm, Gordon, and Kaufmann.9 pecimens for X-ray diffraction were obtained by crushing the ingots and passing the resulting powders through a 200 mesh screen. Diffraction patterns were made with a powder

Jan 1, 1956

The reduction of titanium tetrachloride to trichloride can be achieved by employing hydrogen and electric arcs. It is possible to produce melts containing up to 50% TiCk in the eutectic mixture of LiCl/KCl by striking a D.C. arc at the surface in the presence of hydrogen and TiCl. vapour. If the electrode IS made to just penetrate the surface of the salt mixture, a hot zone results from the' high resistance contact with both lower chlorides and sintered titanium may be produced. The sintered metal forms just below the melt surface while the trichloride forms at the gaslIiquid junction.The "hotspot cathode" appears to offer a solution to the problem of producing coherent deposits as the spong'e metal can 'be continuously withdrawn in a similar manner to the "calcium process".INTRODUCTIONConsiderable interest has been shown for some years in the possible development of a cheap electrolytic process for the extraction of titanium metal, since a method using simple materials and cheap electric power would materially reduce the cost of production. Even when cheap starting materials are used, however, there exist several general difficulties in the operation of plant which both limit the speed of production and increase the cost of the product. It happens that most of the techniques so far tried produce a powder as cathodic deposit, and when this is the case the following difficulties arise:1. The whole contents of the bath must be treated with solvent in order to extract the 'metal powder which may itself tend to oxidise, and thus become contaminated.2. Fine metal powders, which often contain residual entrained salts, are less easy to consolidate by arcmelting than metal sponge.

Jan 1, 1956

By S. Yukawa, M. J. Sinnott

A high resolution autoradiographic study of the diffusion of a nickel isotope (NP3) into copper in the temperature range of 650° to 925°C, with particular emphasis on grain boundary diffusion, has been made. The extent of grain boundary diffusion is a function of the grain boundary angle and the diffusion temperature. The ratios of the grain boundary diffusion coefficient to the lattice diffusion coefficient ranges from 104 to 105. The activation energy for grain boundary diffusion decreases with increasing grain boundary angle. STUDIES and reviews&apos;-8 of metallic diffusion have indicated that grain boundary diffusion is a common phenomenon but quantitative studies of the many variables involved are not numerous. The present work was concerned with determining the influence of the crystallographic orientation of the grain boundaries and the temperature on the extent of boundary diffusion of nickel into copper. The study involved essentially three steps: 1—the production of grain boundaries of known crystallographic orientation, 2—the determination of the extent of diffusion into the boundaries, and 3—the analysis of the resulting data in terms of the usual diffusion concepts. The grain boundaries investigated approximated the simple tilt variety having l° of freedom. They were produced by controlling the solidification from a melt of Cuprovac (a high purity vacuum-melted copper obtained from Vacuum Metals Corp.) of a pair of seed crystals so that the bicrystals of copper produced had a common <100> axis. By rotating one seed crystal relative to the other, a simple tilt boundary was produced. The angle of rotation between the two crystals is the grain boundary angle 8, or what is sometimes termed the misfit angle. In all, some 16 boundaries ranging from 2" to 72" in 5" to 10" steps were investigated. The crystallographic orientations were measured with the use of both X-ray and optical goniometric techniques. The <100> axes in the crystals were found to be parallel within 2" to 3" with the exception of one crystal (8 = 12") in which the axes were 6" from being parallel. All bicrystals showed evidences of sub-grain structures. Laue analyses showed that these subgrains differed in orientation up to a maximum of 2". Because of these variations, and some curvature in the boundaries, the grain boundary angles listed are actually average values and deviate from the 1 o of freedom boundaries. The stripping film technique of high resolution autoradiography was used to detect the diffusion of the nickel isotope into the grain boundaries of the bicrystals of copper. Kodak experimental permeable stripping film with an emulsion layer 5 u thick

Jan 1, 1956

By M. E. Wadsworth, D. R. Wadia

The rate of reaction of cuprite was measured in a series of sulphuric acid solutions, from which oxygen had been excluded, at various concentrations and temperatures. The overall reaction CuzO + H2S04 + Cu " + CuO + H20 + So4&apos; may be explained quantitatively by two simultaneous rate reactions involving not only H+ but also the hydrolytic adsorption of H2SO4. The results indicate the importance of considering surface mass balance relationships associated with heterogeneous surface reactions. T EACHING has long been an important method for the recovery of metals from certain minerals. Many processes have assumed minor importance in modern practice but such operations as the recovery of uranium and present interest in high pressure-high temperature solution of sulphides&apos; &apos; well illustrate the importance of leaching as a unit operation. Little quantitative information is available in a form sufficient to determine the mechanism of solution at the solid-aqueous solution interface for given systems. For this reason, it is important that fundamental studies of leaching processes be conducted so that parameters associated with such surface reactions may be understood and correlated. Cuprite was chosen for this study as a result of a recent investigation carried out at the University of Utah on ores of the Ray and Chino Mines Divs. of the Kennecott Copper Corp. These sulphide deposits contain sufficient oxidized minerals, such as cuprite, malachite, and azurite, so that recovery of metal values contained in the oxidized fraction is of primary interest. Of these oxides, cuprite (Cu,O) is the most interesting, since it dissolves in sulphuric acid by an oxidation reduction couple resulting in the formation of 50 pct metallic Cu and 50 pct cup-

Jan 1, 1956

By H. Kenworthy

[Experimental studies were made to develop a laboratory technique for direct removal of cadmium and germanium from sphalerite concentrates. Cadmium- and germanium-bearing concentrates from the Illinois-Kentucky fluorspar field were sound to be, amenable to an inert atmosphere fuming process for removing these two moats in the form of gaseous sulfides. Treating the condensed fume by pyrometallurgical methods upgraded the material end provided a means of partly separating the constituents. Cadmium was concentrated about 35:1 arid germanium about 300:1. The extractive investigations were supplemented by vapor-pressure studies on the sulfides of germanium to obtain fundamental data for larger scale laboratory conditioning and control when treating the zinc concentrates. Vapor-pressure curves were developed for synthesized monosulfide and disulfide The results of these- investigations indicate the possibility of significantly increasing the recovery of cadmium from zinc concentrates. Comparison with present recovery of germanium cannot be made, since commercial recovery data arc not available.]

Jan 1, 1956

By R. Bakish, W. D. Robertson

IN the course of a study of stress corrosion cracking of AuCu,, it was necessary to develop new electropolishing and metallographic etching methods. The techniques are generally useful for Cu-Au alloys, including the AuCu composition in which transformation markings are well delineated. For electropolishing, the only satisfactory electrolyte and procedure that has been found1 has the composition given in Table I. The solution must be vigorously stirred while polishing and the temperature maintained in the range of 55" to 62°C. The electrolyte is very unstable and can be used only for 10 to 15 min after which its color changes and a dark-brown precipitate forms. The polishing time is between 1 and 4 min depending on the initial surface preparation. The use of a hood is recommended to avoid the danger of cyanide gas which may form at one of the electrodes even though the solution is alkaline. The optimum current and voltage conditions for vertical anode and platinum cathode are on the plateau shown in Fig. 1, in which voltage is measured across the cell terminals. At voltages below the plateau, etching of grain boundaries occurs and under some conditions, which have not been clearly defined, octahedral etch figures are observed. For general purpose grain-size determination in polycrystalline alloys, a 3 pct solution of iodine in methyl alcohol is used with excellent results. However, when it is necessary to reveal small orientation differences or concentration gradients in an alloy, the iodine etch is not satisfactory. For this purpose, a highly satisfactory etching procedure was developed during this investigation. It involves the use of the vapor given off by freshly prepared aqua regia. The solution employed is 3HC1 to lHNO, which decomposes in accordance with the reaction HNO, + 3HC1 = NOCl + 2H,O + Cl,. The polished specimen surface is held about 1 to 2 cm above an aqua regia solution for 2 to 10 sec depending on the intensity of the contrast required and the surface is not subsequently washed. The results obtained with a coarse grained cast structure are shown in Fig. 2. Subgrain boundaries in a single crystal and concentration gradients within the boundaries are developed by the same treatment with the results shown in Fig. 3. Obviously, any conclusions regarding structure-dependent properties will be modified by the pronounced heterogeneity, which is not clearly evident when more conventional methods are used. Interesting structural details are also revealed by treatment for 4 hr at 850°C in unpurified tank argon. Fig. 4 shows a pattern characteristic of orientation-dependent oxidation.

Jan 1, 1956

Jan 1, 1956

By D. S. Bloom

RECENTLY a report has been published on an investigation of the MO-RU system by E. Raub.&apos; In this report it is stated that below approximately 1200°C the system consists of two terminal solid-solution phases and the intervening two-phase field; at 1200°C and above, an intermetallic compound labeled Mo,Ru, makes an appearance. Along with some other little known systems in which it was considered possible for a u phase to form, the Mo-Ru system had been under investigation in this laboratory. Since molybdenum and ruthenium have very high melting points and also since ruthenium is expensive, the investigation was confined to X-ray diffraction by sintered powder compacts. The compositions which were studied were (in atomic percentages): 75 Mo-25 Ru, 67 Mo-33 Ru, 50 Mo-50 Ru, and 25 Mo-75 Ru. All compacts were made from the pure powders, and no chemical analyses were attempted. Each compact weighed about 5 g. All annealing was done in evacuated Vycor capsules, and even though the capsules completely collapsed at 1250°C, they still admitted no air. The results of this investigation in general corroborate the work of Raub. Up to 1150°C the two terminal solutions and the intervening two-phase field were found, and at 1200°C and above an intermetallic compound was found. However, the composition limits of the compound were estimated to lie close to 70 atomic pct Mo rather than 62.5 atomic pct Mo as Raub had reported. At least the X-ray diffraction results indicated that the 75 atomic pct Mo specimen consisted of the molybdenum solid solution plus the compound, while the 67 atomic pct Mo specimen consisted of the ruthenium solid solution plus the compound and the equiatomic composition contained only very little of the compound. The most interesting observation, however, was that the diffraction pattern of the compound was similar to that of the well known u phases, except that unusually large lattice constants were indicated. The d-values, or interplanar spacings, of the diffraction lines (as produced by filtered copper KCX radiation) of the compound are given in Table I, as determined from specimens annealed at 1250°C for 9 hr and then quenched in water. Also shown are the lines of the Mn-Mo u phase as given by Decker, Waterstrat, and Kasper,&apos; the lines of the Fe-Mo a as given by Goldschmidt," and the lines of the Mo-Ru phase multiplied by constants in order to make comparison with the Mn-Mo and Fe-Mo patterns easier. These results indicate that the compound in the Mo-Ru system is apparently isomorphous with the other o- compounds. The rather large lattice constants of the Mo-Ru a phase are acceptable in view of the comparatively large size of the constituent atoms. The data in Table I for the Mo-Ru compound check quite well with those given by Raub, not shown here, though there are some discrepancies between the two sets of data in the estimated intensities of a few lines. Although very little is known at present about this u phase, there are some things which may be pointed out, mainly in comparison with other better known u phases. Even though molybdenum and ruthenium are in the same columns in the Table of Elements as chromium and iron, respectively, the Mo-Ru u phase contains much more molybdenum than ruthenium, while the Cr-Fe u phase centers around or very nearly around the equiatomic composition; furthermore, the Mo-Ru u is stable only above approximately 1200°C, but the Cr-Fe u is stable only below about 825 °C. With respect to its being unstable below 1200°C, the Mo-Ru u is similar to the other binary molybdenum u phases in the Co-Mo and Fe-Mo systems. Similar to the latter two systems, the Mo-Ru u apparently exists over a rather narrow composition range, whereas the Cr-Fe u at lower temperatures is stable over a much wider composition range. The Mo-Ru u thus is closer to the other molybdenum u phases than to the Cr-Fe cr phase. The most striking feature of the Mo-Ru u phase, however, is the absence of any of the transition elements of the First Long Period.

Jan 1, 1956

By A. L. Engel

Production of chromite in California has been from many small, high-grade mines. The opening of the Purchase Depot at Grants Pass, Oreg., in 1951 has stimulated chromite mining in California, and a large number of properties are being reexamined as there is a possibility that some low-grade ores from many of these properties can be beneficiated to meet the purchasing schedule. The Bureau of Mines in its program of conservation is continuing ore-dressing tests on chromite ores to better evaluate their potential. This report is a compilation of preliminary concentration tests on samples from five different properties in California. The concentration tests were made on ores from the David mine, Butte County, the Seiad Creek mine, Siskiyou County, the High Plateau mine, Del Norte County, Bud&apos;s mine, Tuolumne County, and tailings from the Miller concentration plant in San Luis Obispo County, Calif., to determine the possibility of beneficiating these ores so that they will meet the specifications for the Government stockpile.

Jan 1, 1956

By N. J. Grant, C. Stein

A more complete determination of the chromium-rich portion of the Cr-Ni phase diagram was made, based in part on resistivity measurements. The existence of a eutectoid reaction at 1215°C,made,based in addition to the previously reported eutectic reaction at 1343°C, was confirmed. Metallographic studies, lineal analysis, and diffusion-couple evidence were utilized to support Metallographicand extend the findings of the resistivity measurements. Delineation of the a chromium solvus line shows that the maximum solubility of nickel in a chromium decreases rapidly from 25 wt pct Ni at the eutectoid temperature to 16 wt pct. Ni at 950°C. IN recent years alloys of high chromium and nickel content have become of more interest as better performance of metals at higher temperatures is sought. It has become increasingly important, therefore, that the Cr-Ni binary diagram, which is composed of two of the elements commonly found in many high temperature alloys, be known more accurately. In particular, the chromium-rich portion of this diagram has for a long time remained incompletely determined and has been reported in the literature with a great deal of conflicting evidence. In general, electrolytic chromium of nominal purity was used by most of the earlier workers, who, except for Jenkins et al., made no further attempt to purify the metal. In the present redetermination of the chromium-rich portion of the Cr-Ni phase diagram, every effort was made to use the purest component metals available and to retain this purity throughout the preparation of the alloys and their subsequent handling. Early work by Voss, Bain," and Phebus and Blake4 indicated that the Ni-Cr binary diagram was a simple eutectic system with rather extensive terminal solid solutions. Later, Nishigori and Hamasumi," Tasaki, Weaver and Jellinghaus,&apos; Matsunaga, and Jette, Nordstrom, Queneau, and Foote attempted to determine the limits of the phase fields. Except for Jette and coworkers, the other investigators agreed that the temperature of the eutectic reaction occurred between 1320" and 1340°C and at a composition of 50 or 51 pct Cr. There was, however, considerable disagreement as to the melting point of the chromium-rich alloys and the limits of the solid-solution fields. As a result of the studies of Jenkins et al., the liquidus and solidus curves up to 80 and 90 pct Cr, respectively, were outlined. In addition, the solid-solution phase fields at higher temperatures had been investigated and showed only two phases. The boundary of the chromium-rich a phase was not determined precisely according to these authors, but indications were that it tended to confirm the earlier work of Nishigori and Hamasumi. A more recent investigation by Taylor and Floyd,&apos;" using X-ray methods, essentially corroborated the diagrams proposed by Jenkins et al., and by Wise and Eash (see Fig. 1). Again, no indication of a third phase in the chromium-rich portion of the diagram appeared. The earlier observations, however, are not substantiated by the modifications to the Ni-Cr binary diagram proposed by Bloom and Grant." In the investigation carried out by Bloom and Grant, X-ray methods showed that an eutectoid reaction existed at approximately 1180°C, in addition to the eutectic reaction at 1343°C (see Fig. 1). Their determination of the melting point of pure chromium was 1930°C (later revised to 1903"C)." Experimental Procedure and Results The chromium used for this study was electrolytic chromium, made available by the United States

Jan 1, 1956

By W. M. Fox, D. P. Detwiler

IN the course of research on semiconducting inter-metallic compounds, it became necessary to obtain gallium metal of greater purity that that available commercially. Several methods were considered for further purification, including acid leaching,&apos; fractional crystallization,&apos; and zone-refining.3-5 The method of fractional crystallization was discarded as being equivalent to zone-refining in purification but inefficient in material and time. Both acid leaching and zone-refining were tried, and the method finally adopted is a combination of the two. The acid leaching technique has been reported&apos; to produce gallium in which no impurities are detectable spectroscopically. Although this method is very effective in removing oxides and surface contaminants, semiconducting material made of gallium subjected only to leaching indicated little reduction in the concentration of metallic impurities. Zone-refining, however, appears very effective in removing trace metallic impurities, but comparatively ineffective in removing the surface oxide film. Consequently, the method evolved consists of acid leaching to thoroughly clean the surface, followed by zone-refining to remove metallic impurities. The low melting point and relatively high thermal conductivity of gallium introduce some difficulty in maintaining frozen and molten zones in zone-refining. To accomplish this, it is found necessary to reduce the effective ambient temperature by circulating ice water in coils about the regions that are to be kept frozen, while heat is supplied to the molten regions by resistance coils. The power supplied to the heating coils is regulated by a constant-voltage transformer and a variable autotransformer. Both heating and cooling coils are mounted on a transite base. The gallium ingot is held in a closed pyrex tube sliding inside the heating and cooling coils, the reciprocating method of Tanenbaum et al. being employed to move the molten zones through the ingot at a rate of 2 in. per hr. This apparatus is shown in Fig. 1. The results of a spectroscopic analysis f a zone-refined ingot, as well as of the material as-received and after acid leaching, are shown in Table I. The ingot was 32 cm in length, and received 37 molten-zone passes, the molten zone being about 4 cm long. The only impurity found was lead, the following elements being reported also as checked but not found in the pure material: Al, Sb, As, Ba, Be, Bi, B, Cd, Ca, Cr, Co, Cb, Cu, Ge, Au, Fe, Mg, Mn, Mo, Ni, Pt, Si, Ag, Na, Sr, Sn, Te, Ti, W, V, Zn, and Zr. There thus appears no indication of pickup of Al, Mg, or Si from the pyrex boat as reported by Zimmerman&apos; in his fractional crystallization. Thus it appears that definite removal of lead from gallium occurs during the zone-refining process. It also may be concluded that a more sensitive analytical procedure than spectroscopy is required to evaluate quantitatively the purity of zone-refined metals. One such procedure which is proposed for use in the near future is the measurement of very low temperature resistivity. Although this will not identify the impurities present, it offers a very sensitive check of total impurity. Acknowledgment This work was supported by the Air Research and Development Command, United States Air Force.

Jan 1, 1956

By W. L. Dare

This information circular is one of a series the Bureau of Mines plans to publish describing the methods and costs of mining uranium on the Colorado Plateau. The Big Buck mine is one of the larger underground uranium-vanadium ore mines on the plateau. The mine is about 39 miles southeast of Moab in the Big Indian mining district, San Juan County, Utah. The Big Buck claims were located late in 1947, when uranium mineralization was discovered in the Cutler formation at its outcrop along the escarpment that forms the west side of Big Indian Wash. Charles A. Steen made the first major discovery of uranium ore in the Chinle formation in the Big Indian mining district on July 6, 1952, when 14 feet of high-grade uranium ore was encountered in a diamond-drill hole drilled on his Mi Vida claim. The Big Buck ore body now being mined by Standard Uranium Corp. is a southeast extension of Steen&apos;s original discovery.

Jan 1, 1956

By D. W. Frommer

The investigation reported in this paper is one of several included in a broad program of developing new or improved concentration processes for the oxidized and partly oxidized deposits of lead and zinc, A sample from the Playter lease, Newton County, Mo., containing pyromorphite was successfully concentrated by fatty acid flotation to a grade of over 62 percent lead. Owing to the presence of a high content of slime-size values, the overall recovery of lead at that grade was limited to 44 percent. DESCRIPTION AND HISTORY OF PROPERTY The mineral pyromorphite is a chlorophosphate of lead containing 76.4 percent lead, and, although it occurs frequently in association with other lead minerals, it is considered a minor ore mineral of lead. The manner of occurrence of oxidized lead minerals, including pyromorphite, which frequently are no larger in grain size than the clay with which they are found, militates both against development of a simple beneficiation process and high recovery. The profitable exploitation of such deposits depends not only on a successful treatment procedure but a highly favorable metal market as well. For these, and perhaps other reasons, very little research has been done on the recovery of pyromorphite from its deposits.

Jan 1, 1956

By C. E. Lesher

Two processes for agglomerating fine sized ores with low temperature coke are described. One process (Orcarb) agglomerates ores with limited amounts of carbon; the other (ore-carbon pellets) pelletizes fine sized ores, using low temperature cokes as the binder. Data are presented on the products obtained when taconite, magnetite, and hematite concentrates and several titanium oxide ores were used. REDUCTION of finely divided oxide ores has long been a major metallurgical problem. Various methods of agglomerating, notably briquetting, sintering, nodulizing, and pelletizing, have been developed and are in industrial use. Carbon is the usual reducing agent for oxide ores and attempts have been made to agglomerate fine ores with coking coal in order to get the metallurgical advantages of intimate contact and increased particle sizes suitable for subsequent smelting or reduction.1-3 For the past three years, research has been in progress on two processes for combining fine sized ores with reactive carbon in the form of low temperature coke. By one process, designated Orcarb, the ore is coated with coke carbon in amounts limited to that required for reduction and the result is an appreciable but limited increase in product particle size over that of the original ore. The second process, called ore-carbon pellets, produces pellets of fine ore bound by low temperature coke. The first objective was to develop a process for combining an oxide ore with only enough carbon for its reduction, the amount being that derived from the simple reduction equations. The carbon (that amount theoretically required for the reduction of the oxides in an agglomerate with ore), calculated to CO, ranges from 10 pct for zinc calcines Or phosphate Ores to 21 pct for rutile and 26 pct for silica. The carbon required for reducing iron oxides falls between the extremes—10 and 26 pet&apos; When the carbon in the agglomerate is low temperature coke, reduction by hydrogen may be expected to take place, thus modifying the calculated carbon require- ment. On the other hand, in practice, an excess of reducing agent over that required in theory is normally used. Screen sizes of three iron ores on which the greater part of the experimental work was performed are given in Table I. Most of the testing was done with Freeport (Renton Mine) coal, but Pittsburgh and Elkhorn bed coals were also used. The first objective was to agglomerate the ore with sufficient low temperature coke to provide carbon for reduction, i.e., in the range from 10 to 25 pct. This was accomplished by preheating the ore, mixing with pulverized coking coal, and completing the coal carbonization in a plain steel rotating retort. The pilot retort, as it is now constituted, is shown by diagram in Fig. 1 and photograph, Fig. 2. Ore is fed into the upper kiln by a screw; it is heated to 900° to 1100°F by direct flame and it is then discharged into an insulating hopper from which it goes

Jan 1, 1956

By A. C. England, William F. Haney, Paul B. Crawford, Bobby L. Landrum

The creation of unsymmetrical vertical or horizontal fractures in a producing well will result in a unique distortion of the normal shut-in pressures existing at the four surrounding wells. An electrical model study has been made to show how the shut-in pressures at the wells surrounding the fractured producing well may he used to estimate the size and orientation of vertical or horizontal fractures. The pressure differences at the four surrounding wells are recorded during production from the fractured well. The resulting pressure dato are matched from a table of several hundred possible fracture combinations. The table refers to the figure showing the effective size and orientation of the commercially created fracture. INTRODUCTION The creation of commercial fractures about oil and gas wells has led to considerable speculation as to the size and shape of the fractures. It is important that the size and shape be known in certain instances, especially when pressure maintenance programs are to be initiated. It was shown that if knowledge of a vertical fracture could be found that such information may be utilized in planning a waterflooding or gas cycling program and that in some cases the fractures might be utilized very effectively.&apos; Other work showed that it may be desirable to create "pancake" fractures in certain reservoirs but that they should exist in a desirable range.&apos; If the fractures are too large, they should be plugged prior to initiating a pressure maintenance program. If an irregular shaped "pancake" fracture is created, it is desirable to know the orientation of this fracture because similar but unreported studies have shown that "pancake" fractures may or may not substantially affect the sweep efficiencies and performance of the flooding or cycling program. Consequently, it may be desirable in some instances to estimate the effective size and orientation of the fracture. ANALOG An electrical model was used in making this study. The electrical model consisted of a circular reservoir approximately 8 in. in diameter, 1 in. thick and was filled with a dilute salt solution. A copper band formed the periphery of the reservoir. A vertical fracture was simulated by a copper strip soldered to the wire well located in the center of the reservoir. Vertical copper strips of various lengths and orientation were soldered to the wire well to represent vertical fractures in the reservoir. In studies reported here on vertical fractures it was arbitrarily assumed that two fractures originated at the well and extended out into the reservoir. An electrical potential was imposed between the wire well and the periphery of the tank. Plots of the iso-potentials are shown in Figs. 1 through 9. This model provides the steady-state isopotentials existing in a uniform, homogeneous circular reservoir having a vertically fractured well at its center. The permeability of the fracture is much greater than the permeability of the matrix proper. The effects of gravity are neglected. In preparing Tables 1 and 2, four symmetrically located unfractured wells were assumed to exist around

Jan 1, 1956

By J. D. Zetterstrom

This report supplements an earlier publication on lightweight aggregates of North and South Dakota.3/ The purpose of the investigation was (1) to study the expansion characteristics of large samples of Dakota clays and shales in a 12-inch by 15-foot rotary kiln; and (2) to improve the laboratory bloating test as a tool for predicting the suitability of samples for the rotary-kiln process. This was done by comparing results of the laboratory and kiln tests.

Jan 1, 1956

By G. Bhat, J. F. Libsch

lsoembrittlement curves depicting the influence of time and temperature in the range 800&apos; to 1260°F (425&apos; to 680°C) on the development of embrittlement in a commercial chromium alloy steel and a commercial molybdenum alloy steel are presented. Two distinct regions of embrittlement occur in the chromium alloy steel: I—at 800&apos; to 1000°F (425&apos; to 540°C) and 2—in the region just below the lower critical temperature. Embrittlement is most pronounced at 800&apos; to 1000°F, decreasing very rapidly with increasing temperature above this region, only to increase again as the lower critical temperature is approached. The data suggest two distinct modes of embrittlement with possible superposition of the two modes at extended embrittling times in the temperature range 1100° to 1150°F (590&apos; to 620°C). While the molybdenum alloy steel shows little susceptibility to embrittlement at 800&apos; to 1000°F (425&apos; to 540°C), considerable embrittlement may occur just below the lower critical temperature. THE subject of temper embrittlement in alloy steels has received considerable attention in the last few years. Points of view on the mechanism of embrittlement differ, however, resulting in part from the incompleteness of the data developed and in part from the speculation regarding the susceptibility of plain carbon steel to temper embrittlement. Libsch, Powers, and Bhat1 carried out short-time embrittling treatments on an AISI 1050 steel and demonstrated that hardened plain carbon steels are quite susceptible to embrittlement when tempered in the range from 850°F (455°C) to the lower critical temperature. The isoembrittlement diagram,&apos; representing the embrittling characteristics of this steel, is reproduced in Fig. 1. It is evident from the shape of the curves shown that embrittlement in plain carbon steel increases progressively with both temperature and time in the embrittling range. A comparison of the isoembrittlement diagram for AISI 1050 steel with that presented by Jaffe and Buffum&apos; for an SAE 3140 steel shows that up to 930°F (500°C) the isoembrittlement characteristics of the plain carbon steel are similar to those of SAE 3140 steel, although the embrittlement is much more severe in the latter steel. Above 930°F (500°C), the rate of embrittlement in the plain carbon steel increases continuously with increasing temperature; whereas, in the SAE 3140 steel, the embrittlement rapidly decreases. The influence of alloying elements upon embrittlement during tempering thus appears to cause a decrease in embrittlement above the region of maximum embrittlement, i.e., 850" to 1000°F. The question naturally arises as to what effect individual alloying elements have upon the embrittling characteristics of the plain carbon steel. Current knowledge on the influence of alloying elements on temper brittleness may be found in the review papers of Hollomon" and Woodfine. Hollo-mon," from the results of other investigators, has shown that, in general, the amount of embrittlement increases with increasing alloy content (except for molybdenum and possibly tungsten and columbium). Jaffe and Buffum," by a comparison of the embrittlement in a plain carbon steel with that of a SAE 3140 steel postulated that the presence of alloying elements in moderate amounts tends to retard the development of temper brittleness. It is difficult to determine what effect chromium has upon temper brittleness, since most of the information available has been based on the combined effect of other elements with chromium, particularly nickel and manganese. However, Wilten, and recently Jolivet and Vidal,&apos; Vida1, and Woodfine have reported that chromium steels are temper brittle, that the embrittlement is reversible with a maximum rate of embrittlement at approximately 975°F (525"C)," and that the susceptibility increases with increasing amounts of chromium. Taber, Thorlin, and Wallacel" have found a large embrittling effect with increasing chromium content in a medium C-Mn-Ni steel. But Hultgren and Chang," from their experiments conducted on synthetically prepared ternary Fe-C-Cr alloys, could not conclude that these alloys are susceptible to temper embrittlement. However, on addition of manganese or phosphorus, these Fe-C-Cr alloys became susceptible, from which fact they concluded that the embrittlement developed in chromium-bearing Fe-C alloys is due chiefly to the presence of these elements. Considerable data are available to show that molybdenum decreases the susceptibility of steel to temper embrittlement. However, its effectiveness in preventing or decreasing embrittlement appears limited to its presence in small amounts. Vidal" has shown that a plain 2 pct Mo steel was susceptible. Hultgren and Chang" also have shown that molybdenum additions in excess of 2 pct to synthetically prepared Ni-Cr steels did not prevent embrittlement. Jolivet and Vidal&apos; and Lea and Arnold found that molybdenum reduced temper brittleness. Lea and Arnold further stated that molybdenum decreased the rate of embrittlement rather than the total amount of embrittlement, whereas Preece and Carter" have shown that the presence of molybdenum greatly reduces the equilibrium extent of the change at a given temperature but does not appear to influence the rate of embrittlement. There appears to be very little information as to how molybdenum by itself affects the temper brittleness susceptibility of a plain carbon steel.

Jan 1, 1956