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By William Mikulas Lars Thomassen, Clair Upthegrove

Little work has been done in the field of the nickel-tin binary system. The complete diagram has been investigated on two occasions, but the results are in very poor agreement. The structure of a compound NiSn and the solubility of tin in nickel have been determined by X-ray methods. Several investigations have been made of the liquidus curve, and the compositions of the eutectics have been determined. A study of the literature, however, shows that there is no satisfactory agreement between the data presented in the various papers. The present investigation was undertaken in an attempt to determine the equilibrium conditions, and to correlate X-ray with metallographic data. The equilibrium diagram was determined by thermal and metallographic means, and the solubility of tin in nickel further investigated with X-rays. Powder diagrams were made of the intermetallic compounds, and three of the structures were partly determined. NO attempt was made to determine the range of homogeneity of the intermetallic compounds. Review of the Literature Vigorouxl prepared alloys of tin and nickel containing 74 and 92 per cent of tin. By treating these alloys with very dilute nitric acid or with sodium hydroxide he was able to separate residues, both of which analyzed 66.7 per cent tin. This corresponds to the compound NiSn and was reported as such. Guillet2 made the first investigation of the complete binary diagram Fig 1) The maximum point of the liquidus is at 43.5 per cent nickel. Several solid solution areas were found, and the compound NiSn was included on the strength of Vigoroux's work. The investigation was

Jan 1, 1937

By H. E. Ellis, O. L. Patterson, Granville Dutton

A large-scale water-injection program for the Holt Bryant reservoir of the Delhi field has been established by means of the new automatic multi-pool analyzer. The objectives of this program were to increase reservoir pressure and eliminate a cross-dip gradient of 200 psi. Pressure increases during the first 15 months of operation have allowed for increased oil production rates of 2,600 BID or 25 per cent. To determine the required water injection it was necessary to predict natural water influx ram. Elimination of the pressure gradients required the water-injection program to account for the fluid migration and pressure interaction between segments of the reservoir. An integral part of the ana1ysis included the determination of in-place volumes of oil and gas. The operation of the automatic multi-pool analyzer in determining the water-injection program is described. New features of the analyzer inc1ude an automatic maferial balance analog and a leart-squares computer for determination of unknown reservoir properties. Operational procedures are sufficiently simple to allow direct use by reservoir engineers on a routine basis. The rapidity and accuracy with which problems may be solved permit repeated ana1yses as a check upon reservoir performance. INTRODUCTION This paper describes the use of a new analog com- puter in determining the optimum injection program for a complex reservoir. The Holt-Bryant (Fig. 1) is the major reservoir in the Delhi field of Louisiana. Production is from the Tuscaloosa at subsea depths of 2,970 to 3,286 ft. The sand dips to the south and southwest from three to five degrees. The reservoir is approximately 12 miles long and varies in width from 1/2 to 2 miles. Various calculations have placed the initial volume of oil in-place in the wide range of 275 to 355 million STB. Two small gas caps were initially present in the reservoir. The Holt-Bryant reservoir was discovered in Dec.. 1944, and was fully developed with 188 producing wells by 1948. After development was completed, an east-west pressure gradient began to establish itself. This

Jan 1, 1957

By Y. L. Yao

The solubility limit of oxygeu in a titanionn at 850°C has been determined by magnetic measurements as 12.5 + 0.5 pct (29.0—30,9 at. pct). Also in the susceptibility-co~centmtion curve, there is n distinct but not sharp maximum at 19.0 * 0.5 z~t pet (40.5--42.1 at. pct), which indicates the presence of the 6 phase. The magnetic susceptibilities of the alloys of the titanium-oxygen system were determined byEhrlich in 1939.' is alloys were prepared by sintiring mixtures of titanium and its oxide at high temperatures. On the titanium-rich side, despite the fact that the alloy compositions he measured crossed two phase boundaries, the limited results obtained

Jan 1, 1960

By C. E. Jr. Reistle

ALL crude oils become more viscous when chilled, but the only oils that congeal and precipitate paraffin to such an extent as actually to cause production troubles are those that contain an appreciable amount of wax. In handling these oils of high wax content, three distinct problems may be encountered before the oil reaches the refinery. The first problem is the precipitation and accumulation of paraffin in the well, either in the oil string or on the face and in the pores of the sand. The second problem is the accumulation of paraffin and the congealing of oil in the transportation lines. The third problem is the precipitation of paraffin and the formation of tank bottoms.

Jan 1, 1927

By Harlan A. Walker

Rock-drill steel has an important bearing on costs in many mining operations, both directly and indirectly. Direct factors include such items as shop expense, steel consumed per ton of ore produced, cost of distribution and the dust hazard. The latter, although no specific amount may be assigned to it, is an ever-present problem, and is receiving increased attention as the science of mining progresses. Indirectly drill-steel performance affects consumption of compressed air, maintenance of drills and drilling speed. The latter, in turn, increases or retards the tempo of mining and development. These factors, while not all inclusive, are preponderant in their importance. Thus it is evident that in an extensive operation drill-steel expense may run to many thousands of dollars and that thoughtful research leading toward more efficient practice is warranted. Experimental Work During the late spring of 1939, experiments were undertaken at Homestake in reducing changes in drill-steel gauge from ? in. to 1/16 in. In drifts and crosscut headings mounted machines were set up and holes were drilled with ?-in. bit-gauge changes and other holes a few inches

Jan 1, 1940

By Harlan A. Walker

Rock-drill steel has an important bearing on costs in many mining operations, both directly and indirectly. Direct factors include such items as shop expense, steel consumed per ton of ore produced, cost of distribution and the dust hazard. The latter, although no specific amount may be assigned to it, is an ever-present problem, and is receiving increased attention as the science of mining progresses. Indirectly drill-steel performance affects consumption of compressed air, maintenance of drills and drilling speed. The latter, in turn, increases or retards the tempo of mining and development. These factors, while not all inclusive, are preponderant in their importance. Thus it is evident that in an extensive operation drill-steel expense may run to many thousands of dollars and that thoughtful research leading toward more efficient practice is warranted. Experimental Work During the late spring of 1939, experiments were undertaken at Homestake in reducing changes in drill-steel gauge from ? in. to 1/16 in. In drifts and crosscut headings mounted machines were set up and holes were drilled with ?-in. bit-gauge changes and other holes a few inches

Jan 1, 1940

By Milton E. Wadsworth, J. Brent Hiskey

Galvanic interaction between particulate chalcopyrite (CuFeS2) and copper results in the rapid conversion of chalcopyrite to chalcocite. The effects of temperature, surface area, concentration of sulfuric acid and agitation were systematically evaluated. The kinetics were found to be controlled by a steady-state current flow controlled by the effective anodic and cathodic surface areas involved in the galvanic couple. The experimental activation energy was 11.5 and stoichiometric data and reaction products have been characterized. The overall kinetic system has been evaluated based upon an electrochemical model.

Jan 1, 1974

By C. H. Brehaut, W. N. Taylor, R. S. Douglas, H. A. Shannon

The name for this new method of mining is derived from a composition of Horizontal, Radial, Diamond, and the drilling is from raises. This method, worked out at Copper Mountain, B.C., is believed to be distinct in many features from other known methods. Geology The ore deposits of copper Mountain are related to the copper Mountain stock, which is an ideal example of the magmatic in in that it grades from a basic gabbro at the border to an almost pure orthoclase-pegmatite core. The "contact" ore bodies lie along the contact of the gabbro and an older complex of volcanies and sediment termed the "Wolfe Creek" formation. These older rocks, collectively referred to as greenstone, had been fractured prior to the intrusion of the stock and were highly metamorphosed during the intrusion. The "outlying" ore bodies are somewhat different in character, though a similar structural pattern prevails. It is believed that a deep-seated magma of which the Copper Mountain stock is a part has given off solutions that caused a partial graniti-zation of some of the volcanies. Mining problems are caused further by the presence of a series of soft barren dikes intersecting a great many of the ore bodies, which are about 30 ft. wide, strike north-south, and dip at a high angle to the east; and are further increased by the presence of four major faults, with a great many minor faults running at acute angles from them. Fault zones average 8 ft. in width, and consist of gouge and breccia. They strike northeast and dip steeply to the northwest. The faults cut through the ore zones and the dikes, and continue on into the gabbro. The general mine structure with two types of Ore bodies, bounded by weak walls and intersected by several series of soft barren dikes and major faults, indicated that a method of mining should be devised that would remove the ore at low cost with the least disturbance of the waste walls and dikes. , Theoretical Estimate of Stoping with the Diamond Drill After consideration of various methods, the most suitable one appeared to be horizontal drilling to break the ore in a manner similar to shrinkage stoping Drilling vertical holes or rings from a bench and breaking to an open slot was eliminated because the weak walls of ore, dike or waste would not permit this type of opening. It was then decided to drill either horizontal radial holes from a raise or parallel holes from a slot cut across the ore body. After discussion, the latter method was believed unsuitable, for the following reasons:

Jan 1, 1946

By W. A. Rachinger, C. Graeme-Barber, R. L. Bell, R. C. Gifkins, T. G. Langdon

R. L. Bell. C. Graeme-Barber, and T. G. Langdon (Imperial College. London)— The internal-marker technique developed by Ishida, Mullendore, and Grant has enabled them to make some interesting observations on the role of grain boundary sliding in creep. Certain of their conclusions are supported by our own similar experiments on Magnox AL80 (Mg-0.8 pct Al) specimens containing several markers, full details of which will be published shortly. In particular, we would agree that: 1) Using the internal-marker method, there is little difference between Egb, the contribution made by grain boundary sliding to the total strain, measured at the surface and in the interior of a specimen. 2) The measurement of the change in grain shape during creep leads to an underestimation of the grain strain, and hence an overestimate of Egb.. However, the discrepancies between the values obtained by this method and those obtained using markers are not as great as Tables IV and V of Ishida, Mullendore, and Grant would suggest; see below. The authors' Eq. [I] which is used to compute Egb from the transverse displacement ITt of longitudinal marker lines is not given in the reference quoted,'' where in fact only relations for Egb in terms of the longitudinal displacements of markers were developed. As first pointed out by Gifkins and Gittins,12 a problem arises in the use of longitudinal markers. and we will show that Eq. [1] underestimates Egb in the interior by a factor of 2. In Fig. 12, two grains X and Y have become displaced by the vector AC which lies in the plane of the grain boundary ABCD separating them. A longitudinal marker has been split by this displacement into the two parts LA and CAW. If these were surface grains the transverse displacement, Ut. could be obtained by viewing normal to the "top" surface. If interior, a section through CD parallel to the top surface would show the same result, provided the longitudinal internal markers delineated planes normal to the top surface. (This is an essential feature of the markers not pointed out in the paper.) The important point is that the quantity Ut tan B (=BE=DF) only gives the elongation due to the one component AB of the sliding. The elongation V/tan 8 (=GD) due to the component AD must be added to produce the total elongation resulting from the boundary displacement AC. If the grain boundaries in a poly crystalline specimen are randomly oriented with respect to the stress axis it follows that In the interior of a specimen the two sums depend for any difference simply on the definitions "top'' and "side". On the surface it is possible that the two sums could differ somewhat. In either event it is clear that the authors' Eq. [I] underestimates Egb, and in the interior, and perhaps at the surface also, the appropriate formula is given by The suggested modification probably makes little difference to the comparison between surface and interior values of Egb where both were obtained from marker measurements. For the estimation of the correction becomes extremely important where the boundary contribution is large. In our own work on magnox, for example, we have obtained values of as large as 70 to 80 pct, under conditions of high temperature and low strain rate. The use of planar markers transverse to the stress axis would simplify the comparison between surface and interior behavior, because measurement of the longitudinal offsets Us of these markers could be summed to give the total elongation di-

Jan 1, 1965

By H. L. Gilbert, C. T. Anderson, W. J. Kroll

In a previous paper,' the use of a split graphite tube resistor as a heater element for high-temperature furnaces has been described. The principal advantages of this type of construction are: I. The quadruple resistance or voltage compared with the top-bottom clamp resistor furnace. 2. Free expansion of the resistor. 3. The ease of protection from oxidation by air. 4. The firmness by which it may be held in the compact split clamp. This construction appeared to be well adapted for the fusion of high melting metals which require fusion in a vacuum. Zirconium metal had previously been melted at the Albany Laboratory of the Bureau of Mines in a vacuum arc furnace on a water-cooled plate, using a movable tungsten top electrode.% When larger furnace capacities were desired, this type of construction proved to have its limitations as the largest tungsten rods available were about 7/8 in. in diameter. The supply of direct current of high amperage for producing the desired arc characteristics was also not available. Considerable difficulty was also found in compensating the atmospheric pressure on the flcxible tubing of the movable electrodc, at the same time keeping its movement sufficiently free to enable the striking of an arc on any part of the metal briquet. Among the various materials used for the electrodes in conducting experiments in the vacuum arc furnace was graphite. It was found that zirconium fused in a graphite cup with a carbon arc was contaminated to only 0.2 pct carbon. It was therefore decsed to melt zirconium directly in graphite crucibles. A high-frequency furnace was first used in the attempt to melt the zirconium in graphite crucibles. The high-frequency heating coil was placed outside a silica tube which was evacuated by means of an oil diffusion pump backed up by a mechanical pump. The graphite crucible was thoroughly degassed at 19oo"C before use. Considerable difficulty was experienced in operating at such temperatures in vacuo because, as shown by Zintl,3 carbon vapor formed and reacted with silica accortling to the reaction: SiO² + C = SiO + CO. The silicon monoxide which is volatile at these high temperatures reacted with the zirconium, thereby contaminating it with silicon and oxygen. The presence of carbon monoxide was detected by means of a gas discharge tube placed in the vacuum system as indicated by the pale blue glow of the tube as soon as carbon vapor started to react with the hot silica. The reaction between the carbon vapor and hot silica was avoided by the use of split cylindrical molybdenum shields which were inserted between the graphite crucible

Jan 1, 1949

By E. Houdremont, H. Schrader, H. Bennek

The different influences exerted by the various alloying elements in iron and iron-carbon alloys give rise to a great number of complexities, which are difficult to grasp. It is important therefore to study any systematic relations that may exist between the effects exerted by the various alloying elements, in order to obtain a general classification and thus a clearer conception of the nature of alloy steels. A systematic survey of the alloys of iron, based on an investigation of the binary equilibrium diagrams, was recently published by Wever. Although his work deals little with properties of importance in works practice, its purpose being rather to point out the theoretical agreement among the types of binary equilibrium diagrams and the position of the alloying elements in the periodic system (atomic radii, etc.), the classification proposed nevertheless also suggests relationships among the properties of the alloys in question, even though the alloys may contain carbon in addition to iron and the alloying element. Wever divided the alloys of iron into one group exhibiting an open or enlarged gamma field and another exhibiting a closed or restricted gamma field, with both groups capable of further subdivision depending upon whether a continuous series of solid solutions is formed, or, owing to the separation of compounds, etc., only a limited series. Thus all alloying elements which with iron form a closed gamma field, a "gamma loop," produce alloys that beyond the composition corresponding to the greatest extent of the gamma loop are composed of ferrite alone at all temperatures. Alloys of this composition accordingly are not susceptible to ordinary heat treatment because of the lack of transformations. Steels of this class may thus be divided into steels that contain less than the critical amount of alloying element, and are subject to heat treatment, and those that contain more than the critical amount of alloying element and are not subject to heat treatment. Thus chro-

Jan 1, 1935

By H. Schrader, E. Houdremont, H. Bennek

The different influences exerted by the various alloying elements in iron and iron-carbon alloys give rise to a great number of complexities, which are difficult to grasp. It is important therefore to study any systematic relations that may exist between the effects exerted by the various alloying elements, in order to obtain a general classification and thus a clearer conception of the nature of alloy steels. A systematic survey of the alloys of iron, based on an investigation of the binary equilibrium diagrams, was recently published by Wever. Although his work deals little with properties of importance in works practice, its purpose being rather to point out the theoretical agreement among the types of binary equilibrium diagrams and the position of the alloying elements in the periodic system (atomic radii, etc.), the classification proposed nevertheless also suggests relationships among the properties of the alloys in question, even though the alloys may contain carbon in addition to iron and the alloying element. Wever divided the alloys of iron into one group exhibiting an open or enlarged gamma field and another exhibiting a closed or restricted gamma field, with both groups capable of further subdivision depending upon whether a continuous series of solid solutions is formed, or, owing to the separation of compounds, etc., only a limited series. Thus all alloying elements which with iron form a closed gamma field, a "gamma loop," produce alloys that beyond the composition corresponding to the greatest extent of the gamma loop are composed of ferrite alone at all temperatures. Alloys of this composition accordingly are not susceptible to ordinary heat treatment because of the lack of transformations. Steels of this class may thus be divided into steels that contain less than the critical amount of alloying element, and are subject to heat treatment, and those that contain more than the critical amount of alloying element and are not subject to heat treatment. Thus chro-

Jan 1, 1935

By A. S. Adams

A GLANCE at the list of papers1 that have been published since 1920 on the general subject of flotation suggests the variety of ideas that exist regarding the underlying cause of the phenomenon. Among these ideas, we find several coherent theories, but none that adequately and completely explain the phenomenon. Ralston2 and Bains3 suggested an electrical theory which has to do with the attachment of mineral particles to a bubble by the attraction of unlike electrical charges. This theory has its root in the fact that a bubble of air in pure water is electrified in such a way that the surface is negatively charged while the body of the water is positively charged. This result, which was first discussed by Helmholtz, also obtains when the water contains anything except a high concentration of hydrogen ions, or ions which are trivalent or tetravalent. The theory also holds that the mineral particles have positive charges on their surfaces, and so there is attachment between bubble surface and mineral particles by the old law of electrostatics, which states that unlike charges attract.

Jan 1, 1928

By Henry Siegmann

HISTORY OF PRODUCTION AND USE In 1899 the consumption of fluorspar in the United States was reported as 16,000 tons. The invention of the open-hearth method of steel manufacture, plus the beginnings of a fluorine chemical industry, pushed consumption of fluorspar to 250,000 tons by 1918. In contrast to these consumption statistics of the past, the most recent statistics available (1972) indicate a total fluorspar usage in the United States of 1.352 million st (Table 15.4D.1). Fluorspar remains the world's cheapest source of fluorine, and its unique properties make the mineral the most desirable fluxing agent for steel refining. The linking of fluorine with carbon in the late 1930s resulted in the production of fluorocarbon, and constant growth in production over the years has formed the backbone of a strong fluorine chemical industry. For example, in 1972 it is estimated that total fluorocarbon production amounted to 2.113 million tons, and that, in this process, over 1.351 million tons of acid-grade fluorspar was consumed. The producers of primary aluminum long have been concerned about the fast dwindling reserves of natural cryolite. They found the solution to their problem by utilizing fluorspar for the manufacture of synthetic cryolite and aluminum fluoride. Nuclear weapons, as well as the growing number of peaceful uses for atomic reactors, constitute a market for uranium hexafluoride. This chemical and chlorine pentafluoride, used as an oxidizer with rocket fuels, are products that are as much a novelty as fluorocarbons were 25 years ago. Judging from past success in the field of fluorine chemistry research, it is safe to assume that the market for these chemicals will grow in the future. Three major industries account for the bulk of the fluorspar consumption: steel refining, fluorine chemical, and primary aluminum production. These industries have had a pattern of fabulous growth in the past, and their future plans point to a continuation of this pattern. It seems logical that the fluorspar usage also should continue its upward trend. Considering the growth of the fluorspar industry since 1899, and the obvious dependence on imports of fluorspar as a raw material, one of the most puzzling aspects of the past has been the apparent lack of coordination between fluorspar production and fluorspar consumption. A few authoritative voices have spoken out concerning the need to expand fluorspar production in order to meet consumption of the future. During World War II, the U.S. Government took positive steps in this direction by authorizing purchases at attractive prices for its "stockpile program." As a consequence, new fluorspar producing facilities were built, not only in

Jan 1, 1976

Furnace Builder. Engineer with extensive experience in furnace building. Position with well-established firm, branching into new fields. Location Ohio. 11-1343. Erecting and Operating Engineer to take charge of erection of gas-producer equipment and to teach customers how to operate such equipment. Location Ohio. Salary $250 per month. R-1339. Assistant Professor in Mining School, for instruction work; must have had experience in ore dressing and metallurgy. Location Missouri. Salary $1500-$2100 per school year (8 mo.). R-1332. Consulting Engineer, familiar with construction of artesian wells to act in a consulting capacity. Location New York City. R-1324. Mining Engineer and Investigator to do non-metallic mineral investigations in both field and office for United States Government. Position will last at least a year, and may become permanent. Location Washington, D. C. Salary $1800-$2700 depending on qualifications of appointee. R.-1317. Crushing Plant Superintendent, cement mill and construction experience essential. Prefer man who has had limestone crushing experience. Location New York. R-1314. Assistant Professor of Coal Mining, must be a graduate of mining engineering and have had some coal mining experience. Location Philadelphia.. Salary $2200 for school year of 10 months. R-1312.

Jan 9, 1919

By Edmund C. Pechin

I REGRET that I am unable to present this subject in definite form and detail. All I shall attempt at this meeting is to lay before you some curious facts, the bearings and explanations of which must be reserved for future consideration. I hope before the next meeting to have carried experiments far enough to furnish a more important contribution to the science of iron metallurgy. The Wickersham process consists in the introduction into the molten metal, as it runs from the furnace, of air from the hot blast. Mr. Samuel Wickersham is the originator of the plan, as applied in practice, although Mr. Martien had the idea a long time ago, and, I believe, .went to England about it. But at that time Mr. Bessemer was coming before the public with his invention, which engrossed the attention of iron-masters, and Mr. Martien accomplished nothing. The principal difficulty in our experiments at Dunbar was to get a practicable runner or trough, through which the molten metal should pass, and in which it should be exposed to the action of the blast. The runner we used was ten feet long, and perforated on the sides to permit the entrance of the air-currents. When we used a cast-iron and fire-clay runner, the heat was so great that before we were more than half done with a run, the lower part of the runner was melted, and we had a magnificent Fourth of July display of fireworks until the blast was shut off. We had to abandon fire clay. The runner with which we have had the best success ,is made of wrought-iron tubes, 2 1/2 inches in diameter, attached to a wrought-iron frame, and lined with a mixture of crushed conglomerate (quartz) and a little fire clay to give it cohesion. The wrought-iron shell curves inward over the upper edges, so as to catch and throw back into the current the flying sparks and particles of metal thrown out by ebullition. With this we have been able to run 12 to 14 tons at a heat with great ease. Mr. Wickersham has since prepared this material (pounded quartz) into a shaped brick or tile, with the necessary perforations for the passage of the air, which promises to answer every requirement for steady working. As regards the improvement in the quality of the iron, there seems to be no question. A large number of practical tests were made in

Jan 1, 1873

By S. G. Lasky

W E seem to have assumed the careless habit in recent years of treating mining geology as synonymous with exploration geology, and exploration synonymous with exploration for new deposits-to be forgetting that mining geology includes also the geologic control or guidance of day-by-day mining operation. In the publicized romantic spotlight of the search for new deposits, we forget the man with the dirty over-alls, grubbing away at the daily tasks of finding new shoots and of helping to keep production up and cost down. During 1949, as in previous years, the resident geologist continued his quiet efficient functioning while the exploration geologist continued to stay in the spotlight-although this time he shared it with what may be called the resource-appraisal geologist. Many broad problems of national import such as tax modification, the operations of the Economic Cooperation Administration, and certain international relations have come up against an unexpected factor lurking in the background, namely, appraisal of world and domestic reserves and latent resources. T. M. Broderick opened the year with his address as retiring president of the Society of Economic Geologists, wherein he analyzed the problems of exploration geology listing among them "the shortcomings of the geologists themselves, of the educators, the mining companies, our Published by permission of the Director, U. S. Geological Survey. technical publications, the Federal Survey and Bureau of Mines, and the property owners."

Jan 1, 1950

By Paul D. Merica

DURING the Dark Ages, when metallurgy was practiced by the alchemists, any unusual or disturbing variation in metallurgical operations was ascribed to the, presence, in the metals or ores, of an evil spirit, and it was necessary to exorcise and drive it out "by suitable incantations. In this day of science and of engineering, things still incomprehensibly go wrong in the metallurgist's work shop. The metallurgist is even now not unwilling to lay the blame for many such experiences at the door of something which intellectually- much resembles an evil spirit, "gas in the metal." The presence of gases in his metal, he knows, occasions him many very definite troubles which he can clearly distinguish and diagnose-why may it not be also responsible for those which he cannot so well understand?

Jan 1, 1931

By Sandford S. Cole, John S. Breitenstein

The recovery of over 80 pct of the vanadium values in titaniferous magnetite from Maclntyre Development,Tahawus, N. Y., was accomplished by an oxidizing roast with Na2O3-NaCI addition. Process description is given for leaching of roasted ore and precipitation of V2O5 and Cr2O8 from leach liquor. THE exploration and development of the Mac-Intyre orebody at Tahawus, N. Y., by the National Lead Co. provided a source of vanadium. Analyses of various composite sections of the drill cores of the MacIntyre orebody were made to establish whether or not the vanadium was constant throughout. Ten drill cores were sampled as 50 ft sections, crushed, and a portion magnetically concentrated. The head and concentrate were analyzed for total iron and vanadium. The results on the concentrates indicated that the vanadium is associated with the magnetite and maintains a close ratio to the iron content. The nominal ratio of 1:25:140 of V: TiO2:Fe was found to exist in the concentrates. Typical value for the vanadium in the magnetite both from laboratory concentration and mill production is 0.4 pct. The recovery of vanadium from the magnetite was investigated in 1942 to 1943. The research program encompassed both laboratory and pilot-plant work on sufficient scale to provide adequate data to establish the feasibility of a full scale plant. The recovery of vanadium from various ores has been reported in the literature and has been the subject of many patents. The literature dealing with recovery from titaniferous ore by roasting is quite limited. Roasting with alkaline sodium chloride, sodium chloride or alkaline earth chlorides, and sodium acid sulphate have been claimed in various processes as effective means.1-8 The reduction of the ore, followed by acid leaching, was another method proposed.'-' "he use of various pyrometallurgical processes for recovery of vanadium in the metal or in the slag has also been extensively investigated, but the results had little application to the problem."-" The separation of vanadium values from subsequent leach liquors and vanadium-bearing solution has been the subject of a considerable number of papers and patents. The most practical is by hydrolysis at a pH of 2 to 3 by acidifying a slightly alkaline solution. Data on solubility of V²O5 and V2O4 in water and in dilute sulphuric acid indicated a solubility of 10 g per liter in water.'" Laboratory Results Magnetite Analysis: Adequate stock of magnetite was provided so that the laboratory and pilot-plant operation was on ore representative of the mill production. The ore was analyzed chemically and examined by petrographic methods to ascertain whether the vanadium was present in combined state or as an interstitial component between grain boundaries. No evidence was obtained which would indicate that the vanadium was in a free state as coulsonite.15 The analysis of the ore was as follows: Fe²O³, 47.4 pct; FeO, 29.1; TiO,, 10.1; V, 0.40; and Cr, 0.2. The screen analysis of the ore on the as-received basis was: -20 +30 mesh, 28.8 pct; —30 +40, 18.9; -40 +50, 9.7; -50 +60, 15.1; -60 4-100, 5.9; -100 + 200, 11.2; -200 +325, 3.7; and -325, 7.2. Roasting Conditions: The prior practice indicated that a chloridizing roast with or without an alkaline salt had been effective on other titaniferous magnetites. On this basis roasts with additions of sodium chloride, sodium carbonate and mixtures thereof were investigated varying the roasting temperature between 800" and 1100°C. Since the ore had shown no segregation or concentration of vanadium, the influence of particle size on the freeing of vanadium by the reagents during roasting was determined. The initial work was on silica trays in an electric resistance furnace with occasional rabbling of the charge. Subsequently, the roasting was carried out in a small Herreshoff furnace to establish the influence of products of combustion on the recovery of the vanadium. The laboratory tests showed that this ore required an alkaline chloridizing roast, in conjunction with a reduction in particle size to less than 200 mesh. When roasted in air at 900 °C with 5 pct NaCl and 10 pct Na2CO³, over 80 pct recovery of the vanadium was attained as a water-soluble salt. The presence of alkaline earth elements gave detrimental effects and care had to be exercised to avoid any contamination of the ore or roast product by such materials. The solubilization of vanadium under the various conditions is given in a series of curves in Figs. 1 to

Jan 1, 1952

Jan 1, 1947