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By W. L. Dare

This report is one of a series published by the Federal Bureau of Mines to describe methods and costs of mining uranium on the Colorado Plateau. The Navajo Uranium Division of Kerr-McGee Oil Industries, Inc., mines uranium from several deposits of carnotite-type ores, which lie buried in the Lukachukai Mountains on the Navajo Indian Reservation, Apache County, Ariz. The country is rugged and isolated Constructing and maintaining roads has been a continuous task. The ore bodies occur within the Salt Wash member of the Jurassic Morrison formation and are similar to other such deposits on the plateau. The current mining activity in the Lukachukai Mountains is a result of uranium-ore discoveries in 1949, although the Navajos undoubtedly knew of the outcrops of yellow uranium minerals long before that time. The ruggedness of the country and the heavy soil cover over much of the surface hampered prospecting, but probably the main reason the ore was not found sooner is that no one took the trouble to look for it in the Lukachukai Mountains.

Jan 1, 1961

By W. L. Price

The intelligent selection of wire cloth and perforated plate for screening surfaces seems a rather confusing subject to the newcomer in aggregate processing. The proper application of various screening surfaces is a complicated one and one could consider himself an expert only after many years of working with all applications. However, part of the subject matter could be simplified considerably for, the average screen user. In this paper an attempt will be made to do this, by presenting some comparative specification data along with cost figures Unfortunately, it is impossible in the limited scope of this paper to give actual service comparison records between different cloths or cloth and plate. Anyone who has considered making actual service comparisons for competing screening media is well aware of the almost insurmountable problems Their solution would form the basis for a separate paper on that subject alone. Therefore, this paper will be limited to comparative data up to the point of installation.

Jan 1, 1961

By R. J. Gajan

As part of its research program on secondary metal refining, the Federal Bureau of Mines has developed a fast method for determining aluminum, iron, copper, cadmium, and lead in zinc-base alloys. The new method is intended for use by trained technicians in laboratories with inexpensive equipment. It can be used either in the analytical laboratories of the many small plants that are characteristic of the secondary metals industry or in laboratories engaged in basic research to improve refining processes. A complete analysis for the foregoing elements can be made in less than 3 hours from a single sample in solution. The method is especially helpful when a small amount of sample is available. Aluminum and iron are determined spectrophotometrically and the other elements polarographically. The new method is now being used for control analysis in metallurgical research, and the results compare favorably with previously used spectrographic methods. Luke and Braun4/ described a photometric method for the determination of aluminum in zinc diecasting alloys in which the aluminum was complexed with Aluminon reagent (ammonium salt of aurintricarboxylic acid), forming a red lake. An adaptation of this method was used for determining aluminum. Beers law is obeyed between 0.01 and 0.06 milligram of aluminum.

Jan 1, 1961

By H. Linder, W. H. Dennen

The graphitic carbon content of soils may be used to detect and delimit subsurface graphitic zones. Spectrographic measurement of carbon in C horizon soils from several areas in the northeastern United States shows good correlation with known graphitic bodies. Bodies of graphite and sulfides are readily located by electromagnetic prospecting methods, but these methods cannot generally discriminate between them. Usual practice, therefore, requires follow-up work on electrically anomalous areas by trenching, drilling, or soil sampling in order to determine the mineralogical nature of the conductor. The efficiency and cost of such follow-up is consequently an important factor in prospecting. The presence of buried sulfide deposits is often reflected in concentrations of metals in the superincumbent soil. Simple chemical tests for such metal concentrations have been developed and applied with considerable success. Bodies of graphite or mixtures of graphite and sulfides are, however, very common and a means whereby buried graphite could be detected by soil testing should provide valuable additional information in the search for ore sulfide and graphite deposits. Graphite is a notably stable substance and should persist in soil above graphite-rich horizons. Microscopic examination of soil samples high in carbon, however, failed to reveal any recognizable graphite fragments indicating a grain size in the clay range. Presumably such small particles would have some mobility in a soil by a translocation mechanism similar to that proposed for the movement of clay particles in a soil profile. Experimental data supports this idea since the boundary between background and anomalous soils carbon values is quite sharp, but the anomalous zone is slightly broader than the graphitic source rock. A simple spectrochemical technique for the determination of carbon in geological materials has been described by Dennen,1 and may be directly applied to soils. A modification of this technique which employs an arcing chamber through which nitrogen is passed is recommended to decrease contributions from atmospheric carbon dioxide. Tests indicate that soils over graphitic zones may be strongly enriched in carbon. The spectrochemical determination of carbon depends upon the formation of the cyanogen molecule (CN) from carbon in a sample and atmospheric nitrogen, under the high temperatures associated with a dc arc. Samples for analysis are dried, lumps broken, and screened. A small portion of the -100 mesh fraction is packed into a copper electrode and excited as the cathode of a dc arc. The band spectra of cyanogen are recorded photographically and the density of the bandhead CN 3883A is measured. The limit of detection of the method is about 0.01 pct C and its coefficient of variation is about 15 pct. Soils, of course, contain carbon in other forms than graphite, and the amount of interference from such sources was examined. The C horizon of several soils from Massachusetts, Maine, and Pennsylvania were found to have a carbon content of 0.3 to 0.5 pct by weight. This content is chiefly due to the presence of carbonates and vegetable matter in the sample and may be readily eliminated, or at least

Jan 1, 1961

By N. J. Grant, Hans Brunner

ThE materials used in this investigation were furnished by the Aluminum Co. of America and consisted of high-purity alurhinum (99.995 pct) and two aluminum-magnesium alloys containing approximately 2 and 5 pct Mg. The compositions of these alloys are listed in Table I. The materials were received as hot rolled 3/8-in. diam rods and were made from the same heats as the materials which were previously used in this laboratory.'j3 The rods were cold swaged to 1/4-in. diam by 1 in. long, and then had two parallel flats machined over the gage length 0.085 in. apart. The test bars were annealed for 10 min at 700° F, and strained 1 pct in tension at room temperature. They were electropolished (80 pct acetic acid; 20 pct perchloric acid, 70 pct concentration) at a temperature of 60°F at approximately 20 v. A grid, transverse or square, spaced 0.2 mm apart, was impressed by rolling a fine threaded screw (128 threads per in.) across the flat surfaces. The depth of the grooves was less than 5 p. For final annealing and grain size control the specimens were enclosed in aluminum foil and sealed in Vycor tubes. Annealing conditions varied from 1 hr at 700° F to 5 days at 1050° F, depending on the alloy content, to give for most of the specimens a final grain size of about 1 mm. This treatment was followed by electropol-ishing as described above. For the test series presented in Figs. 4 and 5 round specimens were used instead of flat ones, and fine machining marks served as marker lines instead of the impressed grid lines. Electropolishing was omitted. The major advantage is that the spacing of the machining marks is only about 1 u as compared to the 200 u of the impressed grid lines, permitting higher precision in strain measurements. Unfortunately the strain annealing necessary for grain size control also resulted in some preferred orientation of the grains. The preferred orientation of three arbitrary specimens was measured by X-ray diffraction methods and the averaged results are shown in Fig. 1. The possible effects of the preferred orientation on the test results will be discussed later. The testing temperatures were 410°, 515", 725", and 940° F, with one exception in the case of the 5.1 pct Mg alloy. Since the solubility limit of this alloy is 520°F, a test temperature of 545°F was cho-se sen instead of 515°F. The selection of the test temperature was based on two considerations: 1) at 900°F and above, extensive grain boundary migration made it more difficult to measure grain boundary sliding; 2) at 400°F and below, there was so little grain boundary sliding that it was again difficult to make precise measurements. The stress was chosen to give a creep rate of approximately 2.7 pct per hr in connection with Figs. 2

Jan 1, 1961

By Robert H. Raring

Viewed abstractly, a mill may be defined as a mineral processing facility located somewhere between the mine and the tailings storage area, Just how mining operations and the demands of tailings storage affect mill design is, the subject of this paper. At the outset, it will be readily acknowledged that no two installations can, or ever will be the same. At one extreme is the bucket line dredge where the distance between the ?mine? and the tailings area is measured in terms of tens of feet. At the other extreme, the large open pit copper mines are frequently spread across twenty, miles or so of countryside with the ore moving to the mill, as exemplified by the operations at Bingham Canyon, Ray, or Ruth - the "upstream" counterparts of Garfield, Hayden and McGill. In each of these cases, mill location was largely determined by requirements for tailings storage and/or water supply.

Jan 1, 1961

By Samuel P. Polack

This report reviews investigations to determine the fire hazard in coal mining when using flammable petroleum hydraulic oils to actuate mining equipment and summarizes research by the Bureau of Mines and industry on fire-resistant hydraulic fluids. Tests were established to evaluate fire resistance and the necessary characteristics to assure adequate service when fire-resistant fluids are used to replace petroleum hydraulic oils. The research was conducted in the laboratory and field trials under actual operating conditions in underground mines. Bureau of Mines Schedule 30 became effective December 17, 1959; the first approval was granted on February 18, 1960, and the twelfth was granted on March 17, 1961. The approvals include nine ready-mixed (by the producer) fluids and seven concentrates to which water is added by the user according to instructions from the producer. Seven synthetic-type fire-resistant hydraulic fluids submitted by two producers are also approved. Over 100 coal mines are now using water-in-oil emulsion-type fire-resistant hydraulic fluids in varying degrees from a trial in one machine to all the hydraulic equipment in an entire mine.

Jan 1, 1961

By G. V. Jere, C. C. Patel

Chlorination of the various constituents of ilmenite by different chlorinating agents in presence of various reducing agents, have been considered on the basis of the standard free energy and standard enthalpy changes as a function of temperature. The standard free energy change considerations show that it is beneficial to chlorinate ilmenite by chlorine in the presence of carbon and also that iron constituent of ilmenite can be preferentially chlorinated by clzlorine, titanium tetrachloride or their mixture. These findilzgs have been corroborated from the published work. METALLURGICAL processes involving the use of titanium tetrachloride have gained in importance because of the use of the latter in the manufacture of titanium metal. Since ilmenite is more abundant in nature than any other titanium mineral, the future of the metallurgical processes depends on the utilization of ilmenite for the production of titanium tetrachloride. In these laboratories, investigations have been carried out on the chlorination of ilmenite under a variety of conditions.1'2 During these studies, it was noticed that 1) preferential chlorination of iron was effected at low temperatures (400° to 600°C) and at low carbon content (6 to 7 pct), 2) carbonyl chloride retarded the chlorination of iron oxides and titania perceptibly, while 3) carbon-tetrachloride, compounds of sulphur and some other catalysts favored the chlorination. Moles3 has found that oxides of iron are chlorinated in preference to titania at high temperatures, while wilcox4 has claimed the preferential chlorination of titania between 1200" and 1500°C. It has been shown in this paper that preferential chlorination of titania claimed by Wilcox is not likely to occur. Daubenspeck and coworkers5,6 have claimed the preferential chlorination of iron by chlorine or by a mixture of titanium tetrachloride and chlorine between 700° and 1050°C in the absence of carbon. Even when plain titanium tetrachloride is employed as the chlorinating agent, pascaud7 noticed the preferential chlorination of iron and other oxides. The purpose of this paper is to explain from thermodynamical considerations, the various chlorination reactions studied so far. ILMENITE CONSTITUENTS AND THEIR CHLORINATION PRODUCTS Although the general composition of the ilmenite mineral is represented as FeTiO,, most of the ilmenites found in nature have variable quantities of TiO2 (44.6 to 64 pct), FeO (4.7 to 36 pct) and Fe2O3 (6.9 to 28 pct).8 The higher content of ferric iron in ilmenites was attributed by Millerg to the presence of arizonite (Fe2O3.3TiO2). But the X-ray studies by Overholt, Vaw, and odd" have shown that arizonite is a mixture of haematite, ilmenite, anatase, and rutile. Except for the anatase, similar views have been advanced by Lynd, Sigurdson, North, and Anderson8 from magnetic, X-ray, and optical and electron microscope studies. The ilmenite ores can, therefore, be assumed to consist of mineral aggregates of ilmenite, rutile and haematite. From the free energy of formation of ilmenite (FeTiO3), it has been shown by Kelley, Todd, and King11 that ilmenite is stable even up to its melting point (1367°C) and would not undergo decomposition into its constituent oxides. Schomate, Naylor, and Boericke12 have found that in the presence of a reducing agent the iron constituent of ilmenite is selectively reduced. The reaction of chlorine with ilmenite in presence of a reducing agent can, therefore, be synonymous with that of the reaction of chlorine with the constituents of ilmenite, viz., TiO2, FeO, and Fe2O3. Most of the reaction products of chlorination of ilmenite in the presence of reducing agents will be in equilibrium with their dissociation products, depending on the temperature. The titanium tetrachloride is, however, quite stable up to 1500°C due to its covalent nature. The equilibrium for the ferric chloride system has been investigated by Kangro and Bernstorff, 13, schafer14 and Kangro and petersen,15 and the results are summarized in Fig. 1, curves a, b, and c respectively. From these results, it is clear that the ferric chloride disociates as follows: 324° to 700°C FeaCl6(g) ?2FeCl2(c) + Cl2(g) [1] 324°to 900°C Fe2Cl6(g) =2 Fe Cl2 Reaction [I] (curve a) occurs in the forward direction to about 6 pct at 400°C but falls off very rapidly with increase in temperature and beyond 600°C, it is practically negligible, perhaps due to the formation of the stable monomer, FeC13(g). As the temperature is further increased, the amount of FeCl,(g) in-

Jan 1, 1961

By J. E. Gray

Before specifications are discussed it may be well to define the term "Mineral Aggregates." Professor K. B. Woods (1) defined "Mineral Aggregate--An aggregation of sand, gravel, crushed stone, slag, or other material of mineral composition used in combination with a binding medium to form bituminous and portland cement concrete, macadam, mastic, mortar, plaster, etc., or alone as in railroad ballast, filter beds, and various manufacturing processes, such as fluxing, etc. " This definition is too all inclusive for the purposes of this paper; therefore, this discussion will be confined to specifications for natural aggregates which means sand and gravel and crushed stone, and limited primarily to coarse aggregate which is aggregate larger than one-quarter inch in size. To the uninitiated, this may seem to be a very limited subject on an unimportant material. However, aggregates are essential in all types of construction. The tonnage and value of these two aggregates produced in the United States during 1959 as reported by the Bureau of Mines were as follows: Sand and Gravel 729,895,000 tons valued at $728,527,000 Crushed stone 581,721,000 tons valued at $824,411,000

Jan 1, 1961

By P. K. Guerrero, N. Arbiter

The correlation of power consumed by a tumbling mill with the dimensions, speed, and load has been attempted by three principal methods. One of these, the torque formula, has been reviewed critically elsewhere.' This approach, while analytical, disregards the individual motion and speed of the tumbling bodies and assumes that the gross geometry of the entire load is sufficient to establish the power requirement. A more general approach, using dimensional analysis, has been applied in this laboratory by the present authors1'1, and more recently by Rose.3 This disregards the internal conditions within the mill entirely and in effect is an empirical procedure for correlating data. Finally, the complete analysis of tumbling mill dynamics as first made by Davis' attempts to develop the power requirement from individual ball and rod paths and velocities. Although Davis' result is applicable only at a single speed for a given size and load it could be useful, since his optimum speed is at the upper limits of conventional tumbling mill practice. Where power values predicted by the Davis equation were compared with actual mill requirements, they were found too low for small mills and much too high for the largest mills. This suggested that the agreement with actual intermediate range requirements might be fortuitous, and the development of the equation was examined critically. The probable source of error was found to lie in an erroneous assumption made by Davis in converting the energy of ball or rod motion to power. With the same approach, but with different assumptions, a modified equation has been obtained which predicts results that are usually consistently high. This is to be expected, since it is assumed that there is no slip between load and shell and no interference among tumbling bodies. Both these effects should account for the difference. Development of Equation: When a cylindrical shell charged with a substantial weight of rods or balls is slowly rotated about a horizontal axis, the load surface first assumes an inclination that gradually increases to a maximum. Continued rotation results in failure within the load, characterized by a sliding of the top layers down the slope and a reduction in the angle of inclination. Further rotation again increases the angle, and the cycle repeats. If the speed is increased, there is continuous load failure and build-up and a continuous stream of rods or balls descends over the upcoming mass, which moves in circular arcs. At higher speeds the up-

Jan 1, 1961

By J. R. Nettle

The purpose of these studies by the Federal Bureau of Mines was to determine the feasibility of refining low-grade hafnium by an inert-gas-shielded molten-salt electrorefining technique to produce a hafnium metal meeting reactor specifications. The techniques were adapted from those used success-fully for titanium electrorefining. Three electrolytes containing hafnium chlorides were developed from which deposits having a Brinell hardness of 170 or below were recovered. A KC1 + NaC1 + HfC14 electrolyte produced deposits in the hardness range of 140 to 165 Brinell. Deposits with a hardness range of from 132 to 152 Brinell were pro-duced from an electrolyte composed of KC1 + LiC1 + HfC14. A third electrolyte composed of NaC1 + K3HfC17 produced deposits with a hardness as low as 139 Brinell. In a fourth electrolyte, composed of NaC1 + K2HfF6, a measure of refining was accomplished, but under the test conditions no metal meeting specifications was recovered; none was softer than 174 Brinell. A number of metallic impurities were reduced in quantity by the electro-refining process, notably iron, which normally was reduced from 250 p.p.m. to less than 50 p.p.m. Magnesium generally was reduced from 680 p.p.m. to less than 80 p.p.m. Manganese content was also reduced by the electrorefining process. Sponge containing 90 p.p.m. Mn yielded deposits containing a maximum of 50 p.p.m.; some deposits contained only 10 p.p.m.

Jan 1, 1961

By E. G. King

Many of the existing thermodynamic values for the titanium halides are estimates, including all the entropies and high-temperature heat contents of their crystalline and liquid phases. This report contains the results of low-temperature heat capacity measurents (which lead to entropy values at 298.15° K,) and high-temperature heat-content measurements of four halides - trichloride, tribromide, tetrabromide, and tetraiodide. The new data are combined with selected heat-of-formation values at 298.15° K. to obtain improved values of the heats and free energies of formation of these halides at high temperatures, thus supplementing the previous data of Kelley and Mah.5/ ACKNOWLEDGEMENTS This investigation was conducted under a cooperative arrangement between the Federal Bureau of Mines and the Department of the Navy, Office of Naval Research. The work was done by Bureau of Mines personnel using Bureau of Mines calorimetric equipment. The Office-of Naval Research supplied the supporting funds and arranged for procuring the samples of the titanium halides. The samples were prepared and analyzed by the Inorganic Chemistry Section, Division of Chemistry, National Bureau of Standards.

Jan 1, 1961

By J. F. Shea, O. F. Tangel

Battelle Memorial Institute participated in a program for the General Services Administration aimed at developing a nickel-cobalt separation process that could be integrated in the Nicaro nickel plant. At the time the programwas being carried out, the Nicaro process was a straight-through operation, in which the ore was reduced and leached, after which the pregnant solution was boiled to produce a so-called "bulk precipitate" which contained virtually all of the nickel and cobalt which had been dissolved in the leaching step. The weight ratio of nickel to cobalt in Nicaro ore is approximately 15 to 20:l. The weight ratio of nickel to cobalt in the finished product had to be 100:l or higher to meet specifications. Because the Nicaro process embodied no nickel-cobalt separation step, the only way that a bulk precipitate of the specified nicke1:cobalt ratio could be produced was to so adjust roasting and leaching conditions that nickel would be selectively leached and most of the cobalt would be rejected with the tailings. The required selectivity, however, was achieved at the expense of nickel recovery, which was 5 or more per cent less than might have been obtained with the existing equipment, utilities, man power, etc., had selectivity been no object. The over-all purpose of the program was to develop a separation step that could be fitted into or onto the Nicaro facilities and which would permit the manufacture of a product that would meet the desired specifications and still permit the recovery of a maximum amount of nickel. Battelle suggested that this might be accomplished by reprocessing off-specification bulk precipitate and specifically suggested the process based on ammonium sulphate leaching followed by hydrogen reduction of the leach solution according to techniques developed commercially by Sherritt Gordon Mines Limited. Such a process would not only satisfy the objectives of the research but would present two additional advantages. (1) It would produce a separate cobalt product which could be further processed into metal, alloys, oxides, or salts. (2) It would yield nickel in metallic form which might be more generally marketable and command a slightly higher price per unit of nickel than the Nicaro oxide product. DESCRIPTION OF THE PROCESS Figure 1 is a flowsheet of the process. The essential features are: (1) Extraction of about 97 per cent of the nickel and about 85 per cent of the cobalt from bulk precipitate by a principal leach with ainmonium sulphate solution (Step A). Extraction of virtually all of

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

By M. J. Saarivirta, P. P. Taubenbla

This paper presents some high-temperature properties of copper-zirconium conductor alloy compared to copper-chromium alloy. Definite superiority of the copper -zirconium alloy over the copper-chromium alloy at high temperatures is shown. RECENT investigations have shown that cold-worked copper-zirconium alloy possesses good room-temperature strength, ductility, and conductivity and maintains most of its strength at temperatures up to 450°C (840°F). As a result, this alloy is now used for many applications, such as commutator segments, resistant welding wheels and tips, rectifier bases, electrical contacts, and so forth. Early investigations1-3 have shown that the maximum solid solubility of zirconium in copper is close to 0.15 pct and the alloy containing Cu-0.10-0.15 pct Zr exhibits the optimum mechanical and physical properties. Results2 have also shown that the alloy has better elevated temperature strength and ductility than copper-chromium and copper-silver alloys. The present investigation was undertaken to learn more about the elevated temperature properties of copper-zirconium alloy and to compare these properties with those of the copper-chromium alloy. WORK PROCEDURE The commercial copper-zirconium alloy, Amzirc was selected for this investigation. Because this alloy is composed of oxygen-free high-conductivity copper and 0.10-0.15 pct Zr, it was believed that possible disturbance from impurities would thus be negligible. Copper-chromium alloys used in this investigation contained 0.40 and 0.70 pct Cr and balance copper. The Cu-0.40 pct Cr alloy was a commercial brand, whereas the Cu-0.70 pct Cr alloy was made from OFHC copper and Cu-5 pct Cr master alloy. It was made in a graphite crucible under argon gas cover and cast. In the preparation of specimens, all three alloys were treated to give the optimum properties; thus the Cu-0.15 pct Zr alloy was solution annealed at different temperatures to determine the desirable solution annealing temperature. It was then cold worked and aged at 375" to 400°C (705" to 750" F). A solution annealing temperature of 1000°C (1830°F) was selected for the copper-chromium alloys because this temperature is widely used in commercial practice. The same alloy was aged at 450°C (840°F) after solution annealing and cold working. It was found that the maximum precipitation hardening of the copper-chromium alloy occurred at this temperature. When aged after solution annealing, the aging temperature was 500°C (930"F) for both alloys. The following properties were determined: 1) Tensile properties as a function of temperature. 2) Effect of solution annealing temperature on high-temperature tensile properties. 3) Stress to rupture strength at 350° and 400°C (660"to750°F). 4) Impact strength. 5) Electrical conductivity and resistivity as function of temperature. 6) Thermal expansion.

Jan 1, 1961

By R. H. Doremus, E. F. Koch

The first carbide phase that precipitates at 120°C from a iron containing about 0.02 wt pct, C was studied with the electron microscope. In both strained and unstrained material the carbide particles appeared to form on the dislocations in the iron, in agreement with the results of the kinetic study in part II. The structure of the carbide was tentatively identified as an expanded a-iron lattice (body-centered tetragonal) with about 0.7 wt pct C. This phase appeared to be metastable and apparently transformed into cementite or epsilon carbide when the iron was over-aged. WhEN a iron containing less than about 0.025 wt pct C is quenched from 700°C to room temperature the carbon is retained in solid solution and precipitates out slowly with time. The morphology and structure of the precipitating phase are still in doubt, two different carbide phases, epsilon carbide and cementite, have been identified, but there is considerable disagreement about the time and temperature at which they appear.1-4 Epsilon carbide seems to form at lower temperatures than cementite, although one group of investigators4 found only the latter phase over a wide range of aging temperatures. Usually these two phases have been identified after aging times much longer than needed to drain the carbon from supersaturated solution, at least for aging temperatures below 200oC. The precipitated carbides have been observed with the electron microscope,'-5 but again most results have come from samples aged much longer than necessary to reduce the carbon concentration in solution to a low value. In this study the carbide phases were observed in earlier stages of precipitation with the electron microscope, in order to learn more about the shape, size, and distribution of the carbide particles. Samples strained small amounts before aging, as well as unstrained samples, were studied, and the structure of the carbide phase was tentatively identified. EXPERIMENTAL "Ferrovac E" vacuum-melted iron, from which the wires for kinetic studies were also made (Refs. 6 and 7 and the following paper) was used for this work. An analysis of this material is given in Table I; it agrees well with the manufacturer's values. The number of inclusions in the iron was very small, as can be seen in the optical micrograph in the following paper. Pieces of iron about 1 mm thick and 5 to 10 mm in diam were used for all the studies except for those in which the sample was strained before aging; then the specimen was a rod 3 to 6 mm in diam and 20 cm long. The samples were held at about 700°C in wet hydrogen for at least an hour to remove residual carbon and nitrogen, after which they were heated to 950" (in the y region) and cooled to room temperature in the furnace. This treatment gave an average grain diam of more than 1 mm, so that the effect of grain boundaries on the precipitation process was negligible. The samples were carburized at 710°C for about 2 hr in hydrogen that had passed over toluene held at -30°C; then they were rapidly quenched into water. From chemical analysis this treatment gave a carbon concentration of from 0.012 to 0.016 wt pct, which is less than the solubility of carbon at this temperature. After quenching, the samples were aged at 120 "C in an oil bath for vari-

Jan 1, 1961

By H. S. Caldwell

Molten zinc, condensed from zinc vapor, was used by the Federal Bureau of Mines to leach aluminum from an aluminum-silicon alloy made by carbothermic reduction of silicious aluminum ores. Zinc requirements were minimized by re-fluxing condensed zinc in a low-pressure, Soxhlet-type distillation unit. The minimum ratio of zinc used to aluminum in the crude alloy was approximately 2:1. When the system pressure was reduced from atmospheric pressure to 100 microns or less, the rate of aluminum extraction increased by a factor of 20. Leaching rates were much higher when the zinc vapor was condensed directly on the crude alloy than when molten zinc was passed over the alloy in the absence of appreciable zinc vapors. Observations indicated higher extraction efficiencies from crude alloys containing greater amounts of iron. Complete extraction was obtained with negligible loss of zinc. Assuming complete removal of zinc, the aluminum products will contain 1 to 6 percent silicon and about 0.5 percent iron plus titanium. The leached crude-alloy residue is a highly friable spongelike material containing about 80 percent silicon, several percent iron and titanium, with the remainder aluminum. This extraction method has been patented (Patent 2,810,637) and assigned to the Government. Research and development investigations are continuing at the College Park Metallurgy Research Center.

Jan 1, 1961

By L. S. Castleman, R. Resnick

The self-diffusion coefficient of columbium has been measured over the temperature range 1535o to 2120°C, using the radioactive isotope Nb95 as the tracer. The data for the temperature dependence of the self-diffusion coefficient are best fitted by the equation D = (12.4 ± 0.8) exp [(-105,000 ± 3000)/RT] cm2/sec. THE increasing need for high-temperature structural materials has stimulated considerable interest in the properties of columbium, since it is a strong, ductile metal with a high melting point—in the vicin- ity of 2450oc.l One fundamental property which has not heretofore been measured is the self-diffusion coefficient. The self-diffusion coefficient plays an important role in theories of oxidatioq2 creep,' sintering4 and other phenomena. Accordingly, the investigation reported in this paper was undertaken to determine the value of the self-diffusion coefficient and its temperature dependence by the use of Mb95.

Jan 1, 1961

By A. E. Gorum, I. Cornet

Fatigrle of ionic crystals has been studied primarily in magnesinm oxide. under cyclic stress dislocations move irrreversibly; they multiply; slip bands form and grow; cracks mucleate and propagnte, and failure occurs. The use of ionic crystals such as MgO is advantageorus in such investigations because they are optically transparent. Individual dislocation Intersections with {100} surfaces may be observed with a standard microscope, using etch-pit techniques. Slip, deformation, crack .formation, and fracture in MgO crystals under cyclic stress are compared with cotrresponditzg processes in metals. ThE effect of cyclic loading in metals has been studied for many years. The appearance of slip lines is readily observed and the ensuing fracture may also be seen. From these observations it is possible to predict the behavior of a material and make an educated guess as to what is happening internally, but the actual changes taking place within the structure are not readily apparent. If one could obtain a material in which the individual glide components could be observed, it would be invaluable in determining the actual slip distribution resulting from cyclic loading as well as the distribution of slip in the neighborhood of a growing crack. Such a material is magnesium oxide. Dislocation arrays may be observed by means of etch pits

Jan 1, 1961

By Frank Parrish

THIS REPORT by the Federal Bureau of Mines presents data on water-supply wells used by waterflood operators in North Texas and shows the distribution of permeable source sediments. Averages of well characteristics, including static fluid levels, working fluid levels, net thicknesses, producing rates, and depths, are presented and discussed. Essentially all water used in waterflooding is mineralized water from consolidated sediments. This study is concerned with the geology and distribution of these mineralized source sediments, whereas previous work in this area was predominantly a study of shallow sources of potable water. Tables, isopachous maps, and electric-log cross sections are included to describe the several source aquifers. In general, water-producing capacity increases with depth of the sediments. Wells completed in Cretaceous sediments 82 to 600 feet deep yield 50 to 600 barrels of water daily, whereas those completed in Pennsylvanian sediments 360 to 4,110 feet deep yield 100 to 7,000 barrels daily. Although deeper formations are used where oil and water are produced conjunctively and where large withdrawal rates are required, insufficient well data prevented mapping of deeper formations.

Jan 1, 1961