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By O&apos, R. G. Meara, B. W. Gandrud

In 1034 the Southern Experiment Station of the U.S. Bureau of Mines in cooperation with the University of Alabama began an investigation of the availability of kyanite ores as a source of raw material for the manufacture of refractories. Under this program, gravity concentration and flotation tests have been made on two varieties of Georgia kyariite ore, mica schist and massive. Most of the attention has been directed to the mica schist ores, as they are more widely distributed and seem to offer greater economic possibilities than the massive ores. It is evident that the preparation of kyanite for use as a refractory material involves other considerations than the mere elimination of impurities. A concentration process that eliminates impurities satisfactorily may have to be followed by some additional treatment, since the final product must be of a coarseness and size ratio that will make it suitable for refractories manufacture. So far in the investigation at the Southern Experiment Station of the U.S. Bureau of Mines only the concentration problem has been considered, and this paper is intended as an interim report. Ores The schist ores contain 1 to 9 per cent of kyanite crystals embedded in mica and quartz, with smaller amounts of graphite, garnet and iron oxide and minor amounts of other heavy minerals. The garnet content varies from a trace to a few per cent. The minerals are easily released by moderate grinding. The size of the kyanite ranges from fine needles to crystals 1 1/2 in. long, 1/2 in. wide and 1/4 in. thick. The garnet, quartz and iron oxide grains have a smaller mean mesh than most of the kyanite. The maximum size of the garnet crystals corresponds to about 14 mesh and that of the sand grains is considerably less. Most of the iron oxide is still finer, for the minus 100-mesh size is greatly enriched in Fe²O3. The massive ore consists of radiating masses of kyanite interlocked with quartz, mica, corundum and small amounts of other heavy minerals.

Jan 1, 1938

By R. C. Hyslop

THE object of this experiment was to obtain a usable set of field curves for determining the susceptibility of rocks with the vertical magnetometer. The need often arises for determining the susceptibility of rocks in the field in order to interpret magnetic anomalies obtained. This is particularly true when diamond drilling has been done and the relation to the surface rocks of the samples taken is desired. Many methods of measuring rock susceptibility have been developed, but in general they require careful shaping of the sample or pulverizing it in addition to delicate laboratory measuring instruments designed for the purpose. The requirements for a practical method for the determination of susceptibilities are as follows: I. There should be as little alteration as possible of the specimen. 2. A minimum of time should be required in the preparation of the specimen and the calibration of the equipment. 3. The equipment used should be portable. 4. An accuracy within the limits of the survey at hand should be obtainable. 5. A means of measuring the remnant magnetism should be available. LABORATORY PROCEDURE With these ideas in mind, the problem was approached in the manner in which Koenigsberger1 developed his method using the principle of the electrical theory of images of Lord Kelvin and applying it to the magnetic case. This solution of the problem states that the apparent change [ ] in the magnetic field intensity due to the proximity of a specimen is given by: [ ] Where k is the susceptibility of the specimen, m the strength of the pole of the needle, and a its distance from the surface of the specimen, as shown in Fig. I.2 This relation is true only for an infinite body and corrections are necessary for a finite body. Koenigsberger used in his work a variometer of special design. He suggested that a Schmidt vertical balance or horizontal magnetometer, as well as some other instrument, might be used. The Colorado School of Mines horizontal torsion magnetometer operates on this principle. In the

Jan 1, 1941

By W. H. Adams

Inasmuch as] the mining of phosphate rock and its transportation has so general a bearing on the great industries of this continent, entering as well into the problem of our trade with foreign countries, it may be useful to place on record the following list of localities from which certain products of a like nature are received by us in a business way, or in which we are interested more or less either by ownership or by competition. As a ready means of comparison, the percentages of the mine products and the deteriorating constituents are given : Coprolite (Cambridge).—This material is obtained from the Upper Greensand formation in Cambridgeshire. The phosphate runs from 50 to 60 per cent., and averages 64 per cent. It contains much carbonate of calcium, but little iron, in the ferric condition. The superphosphates manufactured from the material are permanent and little liable to a revert." They contain from 28 to 35 per cent. of soluble phosphate. Coprolite (Buckingham).—From the same formation as the Cambridge variety, and very similar in composition.. It averages 60 per cent. phosphate. Coprolite (Suffolk).—These coprolites are not so valuable for the manufacture of superphosphate as the two previous varieties, as the iron they contain is in the ferric state, and liable to "revert" the soluble phosphate. The phosphate varies from 48 to 60 per cent., but averages 54 per cent. They are of Tertiary formation. Coprolite (Potton or Bedford).—The average amount of phosphate in these coprolites is about 50 per cent. In some cases they may, however, run up to 60 per cent., and in others may not exceed 45 per cent. They belong to the Lower Greensand formation. The ferric iron frequently is as high as 4 per cent., and the alumina as much. Russian phosphate comes from the chalk, and occurs in carious rounded masses. It contains from 28 to 35 per cent. of phosphate, but may run up to 69 or 70 per cent. Curacoa phosphate is also of very high class quality, giving 80

Jan 1, 1890

By A. S. Koster, G. D. Rieck

X-ray experiments were carried out to show the occurrence of cylindrical texture in drawn tungsten wire. Only a small amount of (110) (110) cylindrical texture could he found in wires of intermediate thickness, i.e., of about 1.5 mm diameter. DRAWN wires of tungsten and other bcc metals like iron and molybdenum show a well-established (110) fiber texture. Now it might be conceivable that in drawing radial stresses remove the randomness of the crystallites around the [110} axis, thus giving a fiber texture of higher symmetry. In the resulting so-called cylindrical textures a specified plane normal coincides with the radius of the wire. Several authors discuss the occurrence of cylindrical textures in bcc metals. ~ieck' found no cylindrical texture in drawn tungsten wires of 165 n diameter. Leber~ states that in tungsten wires of 3 mm diameter a cylindrical {100)(110) texture is developed, which is gradually converted to a normal fiber texture by subsequent drawing. He also reported a definite cylindrical texture at the surface of iron wires. Peck and Thomas3 observed a nonuniform mode of deformation of the grains in transverse sections of heavily drawn tungsten and iron wires. According to Bhandary and cullity4 a swaged iron wire has neither a perfect (110) fiber texture nor a perfect {100}(110) cylindrical texture. It is clear that the concept of cylindrical texture in bcc metals still lacks a firm experimental basis. Leber's eviden~e,~ which seems to be the strongest, rests upon qualitative interpretation of photographs. The appearance of the 110 and 200 lines on the photograph of 3-mm wire, however, can be very well attributed5 to a normal ( 110) fiber texture superimposed on random background; our Fig. 1, giving a Debye-Scherrer diagram of etched tungsten wire of 180 p, is free of cylindrical texture according to all authors, but is quite similar to Leber's diagram. It was therefore decided to use a different method of X-ray texture determination on tungsten wires of diameters where cylindrical textures may be expected.

Jan 1, 1965

By B. W. Gandrud, R. G. Meara, O&apos

In 1034 the Southern Experiment Station of the U.S. Bureau of Mines in cooperation with the University of Alabama began an investigation of the availability of kyanite ores as a source of raw material for the manufacture of refractories. Under this program, gravity concentration and flotation tests have been made on two varieties of Georgia kyariite ore, mica schist and massive. Most of the attention has been directed to the mica schist ores, as they are more widely distributed and seem to offer greater economic possibilities than the massive ores. It is evident that the preparation of kyanite for use as a refractory material involves other considerations than the mere elimination of impurities. A concentration process that eliminates impurities satisfactorily may have to be followed by some additional treatment, since the final product must be of a coarseness and size ratio that will make it suitable for refractories manufacture. So far in the investigation at the Southern Experiment Station of the U.S. Bureau of Mines only the concentration problem has been considered, and this paper is intended as an interim report. Ores The schist ores contain 1 to 9 per cent of kyanite crystals embedded in mica and quartz, with smaller amounts of graphite, garnet and iron oxide and minor amounts of other heavy minerals. The garnet content varies from a trace to a few per cent. The minerals are easily released by moderate grinding. The size of the kyanite ranges from fine needles to crystals 1 1/2 in. long, 1/2 in. wide and 1/4 in. thick. The garnet, quartz and iron oxide grains have a smaller mean mesh than most of the kyanite. The maximum size of the garnet crystals corresponds to about 14 mesh and that of the sand grains is considerably less. Most of the iron oxide is still finer, for the minus 100-mesh size is greatly enriched in Fe²O3. The massive ore consists of radiating masses of kyanite interlocked with quartz, mica, corundum and small amounts of other heavy minerals.

Jan 1, 1938

By R. C. Hyslop

The object of this experiment was to obtain a usable set of field curves for determining the susceptibility of rocks with the vertical magnetometer. The need often arises for determining the susceptibility of rocks in the field in order to interpret magnetic anomalies obtained. This is particularly true when diamond drilling has been done and the relation to the surface rocks of the samples taken is desired. Many methods of measuring rock susceptibility have been developed, but in general they require careful shaping of the sample or pulverizing it in addition to delicate laboratory measuring instruments designed for the purpose. The requirements for a practical method for the determination of susceptibilities are as follows: 1. There should be as little alteration as possible of the specimen. 2. A minimum of time should be required in the preparation of the specimen and the calibration of the equipment. 3. Theequipment used should be portable. 4. An accuracy within the limits of the survey at hand should be obtainable. 5. A means of measuring the remnant magnetism should be available. Laboratory Procedure With these ideas in mind, the problem was approached in the manner in which Koenigsbergerl developed his method using the principle of the electrical theory of images of Lord Kelvin and applying it to the magnetic case. This solution of the problem states that the apparent change in the magnetic field intensity AZ due to the proximity of a specimen is given by: mk AZ = 2a2 Where k is the susceptibility of the specimen, m the strength of the pole of the needle, and a its distance from the surface of the specimen, as shown in Fig. r.2 This relation is true only for an infinite body and corrections are necessary for a finite body. Koenigsberger used in his work a variometer of special design. He suggested that a Schmidt vertical balance or horizontal magnetometer, as well as some other instrument, might be used. The Colorado School of Mines horizontal torsion magnetometer operates on this principle. In the

Jan 1, 1946

By R. C. Hyslop

The object of this experiment was to obtain a usable set of field curves for determining the susceptibility of rocks with the vertical magnetometer. The need often arises for determining the susceptibility of rocks in the field in order to interpret magnetic anomalies obtained. This is particularly true when diamond drilling has been done and the relation to the surface rocks of the samples taken is desired. Many methods of measuring rock susceptibility have been developed, but in general they require careful shaping of the sample or pulverizing it in addition to delicate laboratory measuring instruments designed for the purpose. The requirements for a practical method for the determination of susceptibilities are as follows: 1. There should be as little alteration as possible of the specimen. 2. A minimum of time should be required in the preparation of the specimen and the calibration of the equipment. 3. Theequipment used should be portable. 4. An accuracy within the limits of the survey at hand should be obtainable. 5. A means of measuring the remnant magnetism should be available. Laboratory Procedure With these ideas in mind, the problem was approached in the manner in which Koenigsbergerl developed his method using the principle of the electrical theory of images of Lord Kelvin and applying it to the magnetic case. This solution of the problem states that the apparent change in the magnetic field intensity AZ due to the proximity of a specimen is given by: mk AZ = 2a2 Where k is the susceptibility of the specimen, m the strength of the pole of the needle, and a its distance from the surface of the specimen, as shown in Fig. r.2 This relation is true only for an infinite body and corrections are necessary for a finite body. Koenigsberger used in his work a variometer of special design. He suggested that a Schmidt vertical balance or horizontal magnetometer, as well as some other instrument, might be used. The Colorado School of Mines horizontal torsion magnetometer operates on this principle. In the

Jan 1, 1946

By M. E. Nicholson

The solubility of carbon in Ni-Cu alloys was determined at 1000°C. The factors which limit solid solubility are discussed with particular reference to the influence of electronic factors. The results indicate the extent of solid solubility is a function of the density of states at the Fermi surface. THE solid solubility of an interstitial element is primarily limited according to Seybolt and Fullman1 and Speiser and Spretnak2 by (a) the strain energy produced when the solute atom takes its interstitial position, and (b) the partial molal free energies of the solid solution and the coexisting phases. In several binary systems of a transition and a noble metal, where there are no abrupt changes in strain energy or free energies of coexisting phases, the solid solubility of an interstitial third element drops abruptly to a negligible value at a composition corresponding to a complete filling of the "d-band." Such a decrease occurs in the case of hydrogen in the Pd-Ag system at 60 pct Ag.3,4 The solubility of carbon in Ni-Cu alloys seems to vary in a similar manner as indicated by the embrittling effect of carbon on these alloys. These al- loys are embrittled by slow cooling due to the precipitation of graphite. This embrittlement can be removed by heat treatment if the carbon content is less than the solid solubility limit at the heat-treating temperature. If the carbon content of the alloy exceeds the solid solubility at the heat-treating given temperxture, the embrittlement cannot be eliminated by solution heat treatment.' Since pure nickel has a carbon solubility of 0.25 wt pct6 at 1000°C, embrittlement is easily removed from commercial nickel and nickel-rich alloys, which may contain of the order of 0.10 wt pct C. Embrittlement due to carbon cannot be removed from Ni-Cu alloys containing 70 to 80 wt pct Cu by annealing unless: the carbon content is of the order of 0.04 wt pct CL or less."' Thus, it appears that the

Jan 1, 1962

L. S. Austin, Denver, Colo. (communication to the Secretary) : Mr Hartman says (p. 4 of the pamphlet) that the penetration of air into the crucible of the blast-furnace " is, of course, a function of the diameter of the nozzle." To this I would emphatically take exception. Fig. 1 represents a vertical ideal section of tuyere, cruciblewalls and charge, immediately at the tuyere, in which the currents of air are represented, both in quantity and in direction, by the tortuous black-lines emanating from the nozzle-opening and passing through channels of the least resistance. As an electric current, flowing by various conductors to a common point, is carried in quantity inversely as the resistance of those conductors, so here the air ramifies through the most open cavities or channels, relatively little of it passing where the resistance due to fine materials is great. This figure represents the course of currents in the vertical plane only. As a matter of fact, they pass away in every plane, as opportunity offers. The effect of blocking or decreasing the area of the nozzleopening would certainly only decrease the quantity of air entering by that particular tuyere, without assisting penetration. The large channels (b, b, Fig. 1, for example) would still carry the larger part of the air, while again the smaller channels (a, a, a) would continue small and take no larger percentage of the air than before. These channels momentarily change, however, with the slow descent of the coke. Further on (p. 5), Mr. Hartman describes the dispersive effect of a single lump of fuel. He has only to conceive the entire spaces before the tuyere-nozzles as filled with such lumps, in order to parallel the condition of affairs I have just explained. It is where the large pieces of the charge come down, that the mass is the most open, and the blast passes most freely. On the other hand, wherever the fine ore collects combustion proceeds slowly, because of the smaller supply of air. The

Jan 1, 1899

By Alfred H. Brooks

PetRoleUm seepages are known in Alaska at four localities, all on Pacific seaboard. These, named from east to west, are Yakataga, Katalla on Controller Bay, Iniskin Bay on Cook Inlet, and Cold Bay on the Alaska Peninsula. Besides these, a petroleum residue has been found near Smith Bay on the north Arctic coast of the Territory. At Katalla, Cold Bay, and Iniskin Bay there has been some drilling for oil, and in the first field several productive wells have been opened up. Alaskan petroleum, so far as its composition is known, is a refining oil, with paraffin base and low sulphur content. Most of what is known of the geology of Alaska oil fields is based on the investigations of Dr. George C. Martin, of the United States Geological Survey. A, G. Maddren, of the same service, has recently made a reconnaissance of the Yakataga oil field. The data to be here presented are chiefly taken from the following publications: G. C. Martin: The Petroleum Fields of the Pacific Coast of Alaska, with an account of the Bering River coal deposits, Bulletin No. 250, U. S. Geological Survey, pp. 9 to 27 (1905). G. C. Martin: Geology and Mineral Resources of the Controller Bay Region, Alaska, Bulletin No. 335, U. S. Geological Survey, pp. 112 to 130 (1908). G. C. Martin and F. J. Katz: A Geologic Reconnaissance of the Iliamna Region, Alaska, Bulletin No. 485, U. S. Geological Survey, pp. 126 to 130 (1912). A. G. Maddren: Mineral Deposits of the Yakataga District, Bulletin No. 592, U. S. Geological Survey, pp. 143 to 147 (1914). Katalla Field The Katalla field is marked by a series of seepages and gas springs occupying an east and west belt, about 25 miles in length and from 4 to 8 miles wide. (See Fig. 1.) This zone skirts the north shore of Con-

Jan 1, 1915

By J. J. Reed

The mines of southeast Missouri's Lead Belt have been in operation since 1864, almost 100 years. During this period about 10 pct of the total ore available has been left in place as pillars, and this now represents the best ore reserve left to the older mines. St. Joseph Lead Co. has been investigating various plans of pillar recovery for several years. The example to be described is only one possible approach under a specific set of conditions. Conditions vary greatly in the different areas within the Lead Belt, and the same approach would be entirely inadequate in certain other areas, but there are important sections where this system is clearly applicable. Horizon mining is practiced in the Lead Belt, and stopes may vary from 10 ft to well over 100 ft high. Fig. 1 is a plan view of 6100 stope, the area to be discussed. For these mines this is a small stope, only 10 to 12 ft high. Before any plans were drawn up for pillar recovery, three independent estimates of the pillar grades were made by the mine superintendent, the mine captain, and the mine geologist. After these results were averaged, pillars indicated to be of economic grade were marked for removal as shown. At this stage several alternatives were considered: 1) retreat with caving, 2) concrete replacement pillars, and 3) systematic bolting and retreat. A retreating system with caving was not chosen because the roof was known to be too bad even to permit loading a blasted pillar before caving would begin. Concrete replacement pillars would have been too costly and would have required a large crew, bulky materials, and unwieldy equipment. Systematic bolting was chosen as being most acceptable for the following reasons: 1) Limited area and spans were involved. 2) Only minor modifications to the jumbo would be required for bolting. 3) Only a two-man bolting crew would be needed. 4) Only compact bolting materials would be required. 5) The bolting plan could be modified to allow

Jan 1, 1960

By R. L. Ash, R. R. Rollins, C. J. Konya

An investigation was performed to determine conditions for optimizing the spacing of simultaneously initiated multiple explosive columns. This was done by using models of mortar, dolomite, and Plexiglas with 10-grain mild detonating fuse as the explosive charge. It was desired to simulate blastholes with multiple primers initiated by detonating fuse or when high-velocity explosives are used in low-velocity materials. It was found that optimum spacing between multiple charges was strongly influenced by charge length. At less than optimum charge length, the spacing at which complete shearing was possible between adjacent charges decreased exponentially with a subsequent loss of broken material volume. For charges fired simultaneously, larger burdens and spacings were possible as compared to those necessary for single-crater charges. For each material studied, there was a characteristic optimum charge length and a maximum attainable spacing at any given burden. Proper selection of the spacing distance between charges is fundamental to successful blasting. Its value directly affects the cost of drilling and explosives used per unit of broken material. In addition, the choice of a spacing that is Compatible with a given set of blasting conditions aids in the control of fragmentation sizing, ground vibrations, overbreak, and throw which in turn, influence other production costs. For example, normally loaded blastholes that are spaced too closely invariably promote overbreak and usually give coarse fragmentation. Unless care is taken, airblast and violent flyrock will occur and under certain conditions cutoffs and misfires may result. Too large a spacing, on the other hand, frequently leads to conditions that form bootlegs or toes. The choice of a particular spacicg to use, however, is largely a matter of individual experience and judgment, usually based on trial and error. Very little is known or can be found in the literature with regard to how the spacing between charges is related to field conditions and charge geometry. As a general rule, the firing time sequence of adjacent charges and properties of a material are thought to have the most significant influence on the spacing distance best suited for any given field condition. For example, delayed initiation of adjacent charges usually always requires a closer spacing than when charges are fired at the same time. This should be expected if one considers that the energy normally dissipated and lost in the surrounding ground from charges fired independently would be captured and utilized for breaking material between charges when they are initiated together. Spacing can be extended also when charges are aligned with structural planes of a material, such as jointing, along which shearing is relatively easy. It is customary to relate the spacing (S) between charges to their common burden (B) in the form of a spacing ratio, or SIB. The burden normally is considered as the optimum depth or distance from any single charge perpendicular to the nearest free or open face at which the desired fragmentation and maximum crater yield are obtained. For production blasting, value of the ratio is generally considered to vary from 1 to 2, depending on conditions.1-6 When adjacent charges are fired independent of one another, the value varies from 1 to about 1.4, the closer amount being employed to square corners or produce craters having the ideal 90" apex angle. The larger ratio is the geometric balance value for craters having an apex angle of 135". The basic ideal crater forms in the plane of the charge diameter for charges fired independently are shown in Fig. 1. In the event charges are fired simultaneously, geometric balance in the plane of their charge diameters suggests that a spacing ratio near 2 would be appropriate, as illustrated by Fig. 2. In practice, however, some compromise ratio value must be selected to conform with the specific ground conditions. An example would be where the jointing planes tend to produce 60° or 120° crater angles, the appropriate geometrically balanced charge arrangement being given by Fig. 3. In this condition, the spacing ratio is 1.15, not 1 or 1.4 as suggested for the 90° cratering of independently fired adjacent charges. In view of the foregoing, it would seem logical to assume that whenever charges all having the same burden are fired at the same time, spacing distances always can be greater than those permitted by charges fired independently. In practice this is not the case, however.

Jan 1, 1970

By F. C. Bond

SIZE of grinding media is one of the principal factors affecting efficiency and capacity of tumbling-type grinding mills. It is best determined for any particular installation by lengthy plant tests with carefully kept records. However, a method of calculating the proper sizes, based on correct theoretical principles and tested by experience, can be very helpful, both for new installations and for guiding existing operations. As a general principle, the proper size of the make-up grinding balls added to an operating mill is the size that will just break the largest feed particles. If the balls are too large the number of breaking contacts will be reduced and grinding capacity will suffer. Moreover, the amount of extreme fines produced by each contact will be increased, and size distribution of the ground product may be adversely affected. If the balls added are too small, grinding efficiency is decreased by wasted contacts that are too weak to break the particles nipped; these largest particles are gradually worn down in the mill by the progressive breakage of corners and edges. Ball rationing is the regular addition of make-up balls of more than one size. The largest balls added are aimed at the largest and hardest particles. However, the contacts are governed entirely by chance, and the probability of inefficient contacts of large balls with small particles, and of small balls with large particles, is as great as the desired contact of large balls with large particles. Ball rationing should be considered an adjunct or secondary modification of the principle of selecting the make-up ball size to break the largest particle present. Empirical Equation In 19521,2 the author presented the following emerical equation for the make-up ball size: B - ball, rod, or pebble diameter in inches. F = size in microns 80 pct of new feed passes. Wi - work index at the feed size F. Cs - percentage of mill critical speed. S — specific gravity of material being ground. D == mill diameter in feet inside liners. K - 200 for balls, 300 for rods, 100 for silica pebbles. Eq. 1 was derived by selecting the factors that apparently should influence make-up ball size selection and by considering plant experience with each factor. Even though Eq. 1 is completely empirical, it has been generally successful in selecting the proper size of make-up balls for specific operations. But an equation based on theoretical considerations should be used with more confidence and have wider application. The theoretical influence of each of the governing factors listed under Eq. 1 was accordingly considered in detail, as described below, and a theoretical equation for make-up ball sizes was derived. Derivation of Theoretical Equation Ball Size and Feed Size: The basis of this analysis is that the largest ball in a mill should be just sufficient to break the largest feed particle into several pieces, excluding occasional pieces of tramp oversize. In this article the size F which 80 pct passes is considered the criterion of the effective maximum particle feed size. The smallest dimension of the largest particles present controls their breaking strength. This dimension is approximately equal to F. As a starting point for the analysis it is assumed that a 1-in. steel ball will effectively grind material with 80 pct passing 1 mm, or with F- 1000µ or about 16 mesh. The breaking force exerted by a ball varies with its weight, or as the cube of its diameter R. The force in pounds per square inch required to break a particle varies as its cross-sectional area, or as its diameter squared. It follows that when a 1-in. ball breaks a 1-mm particle, a 2-in. ball will break a 4-mm particle, and a 3-in. ball a 9-mm particle. This is in accordance with practical experience, as well as being theoretically correct. Confirmation of this reasoning is supplied by the Third Theory of Comminution," which states that the work necessary to break a particle of diameter F varies as F. Since work equals force times distance, and the distance of deformation before breaka4e varies as F it follolvs that the breaking force should vary as F½ These relationships are expressed in Table I, with a 1-in. ball representing one unit of force and breaking a 1-mm particle. This establishes theoretically the general rule used in Eq. 1 that the ball size should vary as the square root of the particle size to be broken. Ball Size and Work Index: The work input W required per ton" varies as the work index Wi, and the

Jan 1, 1959

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 Robert Baschwitz, John Chipman

The distribution of silicon between liquid silver and Fe-Si-C alloys has been studied at 1420oand 1530°C. The data are consistent with earlier studies. New data of Hager on the liquidus lines of the system Ag-Si and the distribution data are used to obtain the activity coefficient of silicon in both liquid phases. Data on the heat of mixing in iron permit accurate extension to 1600°C. Equilibrium data involving SiO2 and silicon in liquid iron together with revised data on the free energy of SiO2 are used to fix the activity of silicon in the infinitely dilute solution. The binary system exhibits strong negative deviation from ideality. At infinite dilution ? Si at 1600" is 1.25 x 10'3, and at concentrations up to NSi = 0.4 the slope d InySi/dNSi has a constant value of r; = 13. It is found that logysi in the ternary solutzon is approximately but not exactly the same function of Nsi + NC as of NSi in the binary. The results are consistent with currently available data on the free energy of Sic and its solubility in molten iron. LIQUID solutions of the system Fe-Si-C have acquired considerable importance as the laboratory prototypes of blast furnace hot metal. Equilibrium studies involving such solutions and slags approximating those of the blast furnace have yielded useful information concerning the thermodynamic properties of blast furnace slags. In studies of this kind great importance attaches to a knowledge of the thermodynamic activity of silicon in the solution as a function of temperature and composition. An attempt was made by Chipman, Fulton, Gokcen, and askey' to evaluate all of the pertinent data on this system and to deduce the desired relation between activity, composition, and temperature. These authors published data on the solubility of graphite and Sic in molten Fe-C-Si solutions and on the distribution of silicon between liquid iron and liquid silver. They showed further how the activity of silicon in very dilute solutions in liquid iron could be calculated from equilibrium data involving the molten alloy and solid SiO,. These calculations rested on the published thermodynamic properties of SiO, in- cluding its heat of formation which at that time was recorded as -209.8 kcal. This value has been under suspicion for some time and has recently been replaced by the concordant results from two independent laboratories2,3 which place the heat of formation of a-quartz at -217.6 kcal. This revision necessitates a re-evaluation not only of the activity of SiO2 in slag but also of silicon in molten iron. It is the purpose of this paper, therefore, to recalculate the activity of silicon, and in furtherance of this objective to present new data on its distribution between liquid Fe-Si-C alloys and liquid silver. HEAT OF SOLUTION OF SILICON IN IRON In order to determine the effect of temperature upon the activity coefficient it is necessary to know the heat of solution of silicon in iron as a function of composition. This is found in the data of Korber and Oelsen4 shown in Fig. 1. The curve corresponds to the following equation, which is of a form suggested by Wagner:5 Here AH is the heat absorbed in kilocalories in forming one gram atom of molten alloy from its molten elements and the N's are atom fractions. The relative partial molal enthalpies of the components, each referred to its pureliquid state and defined as zFe = aFe - PFe and zsi = HSi — -psi, are shown graphically. At low concentrations zSi = -28.5 kcal, in agreement with Kijrber and Oelsen's computation. This is in good agreement with the value of -29.3 kcal obtained by Chipman and Grant6 using an entirely different method. ACTIVITY AT INFINITE DILUTION From the known free energy of SiO, it is possible to obtain the activity of silicon in dilute solution in liquid iron from equilibrium studies. The heat of formation of a-quartz is —217.6 kcal and the heat capacity and entropy data are given by Kelley and ~ing.' The free energy of formation of ß-cristo-balite at temperatures above the melting point of silicon is expressed by the following equation: Si(Z) + O2(g) = SiO2 (crist); AF" =-226,500 + 47.50T [I] The value of the deoxidation product for silicon [%Si] x [%O]2 at 1600°C according to Gokcen and chipmans is 2.8 x 10"5, in agreement with results of Hilty and Crafts.9 More recent works of Matoba,

Jan 1, 1963

By C. W. Beattie, R. L. Solter

ALUMINUM-KILLED, low carbon steel sheets are used extensively for severe deep drawing and other difficult forming operations. They usually, but not always, have a characteristic grain structure in which the grains are elongated both in the lengthwise and in the transverse direction. As described by Burns and McCabe,&apos; a typical grain in the plane of the sheet has its two axes in that plane from 1 Y2 to 4 times as long as the axis normal to the plane of the sheet. Rickett, Kalin, and MacKenzieZ have also reported on the recrystallization behavior of such steel. The contrast in grain structures of fully processed sheets of aluminum-killed and rimmed steel is illustrated by Figs. 1 and 2. The elongated grain structure of the aluminum-killed sheet is not developed on all heats or lots of this metal, and studies of the factors controlling and influencing its formation are reported in this paper. Jeffries and Archerb tate that unstrained grains are normally equiaxed, but exceptions are common. For example, if a metal containing a material mechanically obstructing grain growth is subjected to considerable working followed by thorough annealing, it may exhibit grains consistently elongated in the direction of working. Our experiments demonstrate that aluminum-killed, low carbon steel is such a metal, and that the substance mechanically obstructing grain growth is aluminum nitride. The effectiveness of aluminum nitride in inhibiting grain growth has been found to be influenced by the degree of cold reduction, the rate of heating in annealing, the thermal history of the sample before cold reduction, and the residual aluminum content. A correlation between grain shape and austenitic grain coarsening temperature also was indicated and additional experiments demonstrated that aluminum nitride is also the principal cause for the fine grain characteristic of aluminum-killed steels. Manufacture In conventional practice, aluminum-killed sheet steel is manufactured from a low carbon steel containing approximately 0.02 to 0.07 pct residual (HC1 soluble) Al. With the exception of certain samples containing greater or lesser amounts of aluminum, the steels used in these investigations were within the following composition range: C, 0.03 to 0.06 pct; Mn, 0.28 to 0.38; S, 0.017 to 0.032; Al, 0.03 to 0.06; P, <0.01; and Si, <0.01. Properly heated ingots are rolled to slabs about 4 in. thick. After surface conditioning, the slabs are reheated to about 2300°F and hot rolled continuouslv to strip about 1/10 in. thick. The strip rolling is completed at a temperature of 1550°F or higher, and the strip is coiled, usually at a temperature near the lower critical transformation. After cooling, the strip is pickled to remove oxide, cold reduced 40 to 70 pet to final thickness, then annealed to 1250° to 1350°F in 20 to 80 ton charges, the size of which results in slow heating and cooling rates. Effect of Cold Reduction According to Sachs and Van Horn,&apos; the deformations of the individual grains in rolling are similar to those of the total volume. Thus individual grains would elongate in rolling according to the amount of cold reduction imposed. This is true theoretically, but as cold reduction increases the individual grains tend to fragment, and measured grain elongations become less than theoretical. The amount of grain elongation may be described by a numerical rating based on grain counts made by the intercept method. Specimens are polished normal to the plane of the sheet, with the polished surface extending parallel to the rolling direction. After etching, grain intercepts are counted along a 50 mm line on a micrograph of suitable magnification. In random locations parallel to the plane of the sample 20 counts are made and 20 are made in the thickness direction of the sample the average count in the thickness direction divided by the average count parallel to the plane of the sample gives a numerical rating of the grain shape called grain elongation. For example, a grain elongation of 2.00 means that the average grain is twice as long as it is thick. The average of both counts may be converted to grains per sq mm by a nomograph relating intercept counts and grain count. By the same procedure the grain elongation in the plane of the sheet but transverse to the rolling direction may be determined, using transverse metallographic samples. A comparison of theoretical and measured grain elongation was obtained on an aluminum-killed

Jan 1, 1952

By J. F. Martin, L. M. Melnick, R. Rapp, R. C. Takacs

Recent studies on the determination of hydrogen in steel have shown that the hot-extraction method for removing hydrogen from a solid sample is preferable to its removal from a molten sample by vacuum fusion or by fusion in vacuum with tin. A number of techniques are available, however, for determining the hydrogen so extracted. They include: thermal conductivity, gas chromatography, pressure measurement before and after catalytic oxidation of the hydrogen to water and removal of the water, and pressure measurement before and after diffusion of the hydrogen through a palladium membrane. These techniques have been evaluated on the basis of initial cost, maintenance, speed and accuracy of analysis, and applicable concentration range. The results of this study showed that the palladium-membrane technique is best suited for routine use. FOR some time investigators have been concerned with the origin, form, and effect of hydrogen in steel. In such stdies&apos;, the analysis for hydrogen constitutes one of the most important phases. It is quite apparent that the results for hydrogen concentrations in a given steel are dependent on the method of obtaining the sample, storage of the sample until analysis, preparation of the sample, and analysis of the sample, including all the facets inherent in the calibration and operation of an apparatus for gas analysis. There are a number of means available for determining hydrogen. This is a critical study of some of the more common techniques in use today. In most conventional melting and casting methods, hydrogen concentrations of 4 to 6 parts per million (ppm) in steel are quite common. Because of the undesirable effects of hydrogen on steel there has been increased use of techniques such as vacuum melting,&apos; vacuum casting, and ladle-to-ladle stream degassing, which lower the hydrogen content to levels on the order of 1 to 2 ppm. Therefore, the method used for determining hydrogen in steel must be sensitive and precise. In any analytical procedure for gases in metals there are two distinct operations—the extraction of the gas from the metal and the analysis of the extracted gas. To extract the gas from the steel, three methods have been employed: 1) fusion of the sample with graphite at high temperature; 2) fusion with a flux, such as tin, at a lower temperature; and 3) extraction of the hydrogen from the solid sample at a temperature below the melting point of the steel. Fusion with graphite is the least-acceptable method. The blank in this method is higher and more variable than in either of the other two methods. The hydrogen fraction of the total gas composition usually is between 10 and 50 pct; thus, a larger analytical error is possible. The vacuum-tin fusion4 extraction of hydrogen is probably the most rapid method in use today; the extraction time is usually about 10 min. However, with this system a bake-out of the freshly charged tin for 2 hr is necessary and a change of crucible and a charge of fresh tin are required after each day of operation whether one or thirty samples have been analyzed. In addition, frequent checks of blank rates are required since CO and Na are continually being given up by the steel samples dissolved in the tin bath. The composition of the gas in this method lends itself readily to analysis; although the hydroge concentration may fall to as low as 50 pct, more often it is above 90 pct, thus allowing a more precise analysis (because of less interference from other gases). In 1940 ewell&apos; published the hot-extraction method for extracting hydrogen from the solid sample, comparing analysis for hydrogen extracted at 600°C with similar analysis for the gas extracted at 1700°C by fusion with graphite. Good agreement for hydrogen was obtained between these two methods, provided sufficient time was allowed for extraction at the lower temperature. carsone obtained good results in his comparison of this hot-extraction method with vacuum-tin fusion. Subsequent work by Geller and sun7 and Hill and ohnson&apos; has shown that steel samples should be heated to at least 800°C to effect the release not only of the diffusible hydrogen but also of the "residual" hydrogen that may be present as methane. Since the rate of evolution of hydrogene9l0 depends on such factors as sample size and composition, thermal history, and extent of cold work, a fixed extraction time is not possible. Extraction times of 30 min are normal, but 2 hr are not unusual. Induction or resistance heating may be used in the hot-extraction method. With resistance heating the

Jan 1, 1964

By J. Versluys

WHEN a well strikes an oil-bearing layer, the oil has a pressure which is generally sufficient to enable it to rise to near the surface (sometimes above the surface). As soon as a well begins to produce, however, the liquid moves through the pores of the reservoir bed and the pressure in the well becomes much lower than the pressure originally prevailing there. At some distance from the well, however, the pressure in the reservoir bed remains unaltered; thus the pressure of the oil has not only to lift the oil, but also to overcome the friction resistance in the pores. The fact that so many oil wells are gushers is a consequence of the energy accumulated in the gas. In gushing the well acts as a gas-lift. A mixture of liquid and gas (the latter partly dissolved in the former) rises vertically from the oil¬bearing layer through a cylindrical casing to the surface. In time conditions alter and the well ceases to gush regularly, then the gushing can be further promoted by inserting a narrower tube in the well and connecting the top of the oil string to the tubing. If the action in time becomes irregular, the gushing can be kept up for a further period by forcing gas between the two tubes. In the oil fields the term "gas-lift" is used actually only where extraneous gas is applied, as in the last of the stages mentioned. The action, however, is just the same whether the gas exclusively originates from the formation, or is partly applied artificially. Thus by gas-lift we simply mean a vertical tube in which the energy of gas under pressure, and of dissolved gas, is utilized for raising a liquid. In gushing oil wells the pressure is frequently very high and the absorption coefficient 0.4 (expressed in vol. ratio) of the coexisting gas is not particularly high, so that in reality it should be assumed that a considerable portion of the gas, at any rate at the bottom of the gas-lift, is dissolved in the oil. For water-producing wells this is not usually of such importance.

Jan 1, 1929

By Mark Sheppard

DURING the winter of 1937, the writer visited a West Virginia stone, quarry at which the overburden is stripped hydraulically. The quarry is in a bed of limestone, about 200 ft. thick, which outcrops on a hillside above a small river; the quarry face is 175 ft. high. The top of the stone is cut in all directions by erosion channels, which are filled with a tough, red clay. Some of the larger channels are 30 ft. deep and 8 ft. wide, The thickness of the clay overburden ranges from a few inches to 10 ft., the average being estimated as less than 3 feet. The topography of the district is rugged, and the hillside above the quarry face is not suited to the use of the usual mechanical methods of moving dirt. Until hydraulicking was started 10 years ago, the over-burden was dug by hand labor, dumped to the quarry floor and trans-ported to the dump in quarry cars, Cleaning deep channels was a slow and expensive process. When hydraulicking was started, the top of the quarry face was over 200 ft. above the level of the river. The pipe line was carried in a semi-circle around the top of the quarry about 200 ft. from the face and about 50 ft, above it. As there is no adequate supply of water above the quarry, the water must be pumped from the river: As quarrying pro-gressed the pipe line was moved until the discharge points are now over 300 ft. above the river. Water is pumped from the river by a four-stage centrifugal pump having a 5-in. intake and a 4-in. discharge. It is direct-connected to a 200-hp,, 2300-volt, 1760-r.p.m. induction motor. At 1760 r.p.m. the rated capacity of the pump is 750 gal. per minute under a head of 600 ft. The pump is installed in a house of frame construction on the river bank, about 10 ft, above normal water level, which also houses the pump for the mill-water supply. Above the pumps are hoisting hays into which the motors are raised whenever the river reaches flood stage.

Jan 1, 1938

By Arthur L. Flagg

The Elk City mining district of Idaho occupies a position near the geographical center of Idaho county, a region of moderate elevation in the western foot-hills of the Bitter Root mountains. The district comprises an area of approximately 350 Sq. miles, bounded on the west by the Newsome district and on the south by the Dixie and Oro Grande districts. There are no mining districts to the north or east. Elk City, the principal town and the seat of the mining office for the district, is situated in a hydrographical basin surrounded by low hills. The elevation is 4,200 ft. above sea-level. Through this basin flow Elk Creek, Red river, and American river, which unite west of town to form the south fork of the Clearwater. The one township is set out from the Bitter Root Forest Reserve. Though a railroad starting from the Stites terminus of the Clearwater Short Line of the Northern Pacific railroad has been under consideration for some years, the camp is yet without railroad facilities. The projected road would follow the south fork of the Clearwater on easy grades, but would be very expensive to build and maintain. While such a road would greatly benefit those who are now operating in the camp, and in a sligh degree stimulate interest in its possibilities, there is hardly business enough to warrant its construction. At present all supplies and equipment are hauled in by wagon from Stites, a distance of 58 miles, over a wagon road constructed by the State in 1904, following in the main the old Nez Perce trail. While this is not a bad road, it is not all that might be desired. Starting at Stites at an elevation of 1,327 feet above sea-level, the road runs through low hills to Clearwater, a distance of 10 miles. In the next 16 miles the climb is steady until the Mountain House is reached, which is near the summit of Mount Pisgah. This is the highest point passed on the road, having an elevation of 6,500 ft. From the

Jan 1, 1914