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By P. F. Kinyoun

MANY interesting new features are embodied in the latest extension to the open-hearth department of the Bethlehem Steel Co., at Lackawanna, N. Y. Automatic control of the important factors in furnace operation-fuel, air, draft, pressure, slag composition, and of the temperature in various regions of the furnace-has been carried out to a remarkable degree; the human factor is minimized, and the chances for mishaps and irregularities in operation are greatly reduced.

Jan 1, 1937

By Rodolfo V. de la Cruz

The in situ deformability of rock masses is determined by relating the applied load to the radial displacements of points on the borehole wall that are outside of the loaded surfaces. The external displacement method includes the steps in which: a) radial displacement sensors are installed to measure the change in length of a diameter of a borehole; b) unidirectional self- equilibrating pair of forces perpendicular to the direction of radial displacement measurements are applied on opposite sectors of the borehole wall, and; c) using elastic theory, the in-situ deformability of the rock mass can be related with the applied loads and measured radial displacements. The displacements outside the loaded surfaces are comparatively smaller in magnitude than displacements inside the loaded surfaces. These displacements, however, are sufficiently large and can be measured precisely by commercially available linear displacement sensors. Loads are applied by a conventional borehole jack. Existing methods for measuring the in situ deformability of rock masses yields unreliable results due to complex boundary stresses, small and varying contact areas, and the existence of fractures. It was shown that in the external displacement method, the effect of boundary pressure distribution and contact area are negligible. Also, since the displacements measured in the external displacement method were due to materials that are deeper inside the rock mass, borehole fractures have less influence on the calculated deformation modulus.

Jan 1, 1982

IN the extra-mural service being built up by the Engineer-ing Societies Library as its finances permit, an occasional large total charge is incurred for exceptionally protracted services. A western steel company, for example; was charged the unusual fee of $500. They wanted complete informa-tion on transverse tests of steel, and asked the library to compile copies of all accessible records. Weeks -of search-ing and photoprinting produced three volumes of data. Two years afterward the company's chief engineer told the director of the library that the cost seemed high when the bill was paid but that the volumes had been in constant use. The information had been worth thousands of dollars. A client who wishes to pay no more than a moderate fee for services can state to what limit he is willing to go. Thus he may specify that he would like searches made on a particular subject but that he does not wish to exceed $5 or $30- for the information. The library is as willing to perform a small service as a large one.

Jan 3, 1928

By A. W. Ashbrook

There are essentially three main classifications for extractants: acidic, basic, and neutral. The acidic and basic are also referred to as cationic and anionic, respectively. Some extractants are shown in Table 11-1. Acidic Extractants Acidic extractants which are of use, because of cost and/or insolubility in water, are alkylphosphoric, sulphonic, aliphatic monocarboxylic acids and naphthalene derivatives.

Jan 1, 1978

By M. W. Fabjanczyk, E. G. Alexander

INTRODUCTION The purpose of this paper is to summarise development of design processes used in the 1100 oreoody as a result of experience encountered. Design methods have been developed as a result of the history of ground behaviour, free-standing qualities of cemented back fill and mass blasting techniques. This paper contains an historical review of design methods previously described by Matthews ( 1972 ) , Hornsby and Sullivan (1977 and 19781, Kirkby, Blair and Hutton (19781, and Stewart (1980). The reasoning behind design philosphy changes are discussed and placed into context with methods now adopted. The 1100 orebody is Mount Isa's main producer of copper ore (5 million tonnes per year ) . Proven reserves are 120 million tonnes at 3.2% Cu. Location of the 1100 orebody in relation to overall mine geometry was well described by Dayton (1976). Geology The orebody is located in a series of massive brecciated shale lenses, in either a siliceous or dolomitic matrix, surrounded and separated by a uniform shale sequence. The whole formation is truncated at depth by a faulted contact with a greenschist facies metamorphic sequence below (Figure 1 and Figure 2) Mathias and Clark (1976). The breccia is known locally as silica dolomite and contains nearly all the economic mineralisation. Interfingering of shale and breccia often results in irregular boundaries to the silica dolomite and the ore limits. Geometry The geometry of the orebodies is shown by Figures 1, 2 and 3. Figure 3 also shows the location of the copper orebodies in relation to the lead orebodies. Structure Although the orebody is contained within the massive breccia (u.c.s. 150-250 MPa), it is cut by shear zones sub-parallel to the regional bedding (north-south striking, dipping approximately 60o to the west), and diagonally by major transverse faults (Figure A). These major faults have continuity in excess of 300 metres, with varying amounts of displacement up to 200 metres, and are zones of potential movement.

Jan 1, 1981

By Carl Floe

A NUMBER of proposals have been made for the hydrometallurgical recovery of copper from flotation concentrates, but as yet no process has been developed that has demonstrated an ability to compete with the present smelting methods under ordinary conditions. The treat-ment of copper concentrates by hydrometallurgical methods is in general similar to that used in the present electrolytic zinc process and involves roasting, leaching with H2S04 solution, separation of solutions, control of impurities and electrodeposition. While many of these steps are simpler and more readily carried out for copper than for zinc, a number of inherent difficulties have prevented the general adoption of the process. To compete with smelting, the following problems must still be con-fronted, although many solutions for their have been proposed: (1) con-duction of the roast in such a way that leaching will give an extraction of copper comparable to that obtained by smelting; (2) regulation of the ferric iron content of the solutions during electrolysis; (3) disposal of the excess acid regenerated from the sulphates formed in roasting; (4) eco-nomical recovery of the precious metals from the leach residues. The roasting problem is largely one of preventing the formation of copper ferrites, CuO.Fe2O, and Cu20.Fe2O3, which are quite insoluble in dilute sulphuric acid. These ferrites are apparently formed' to a small extent even at low temperatures and above 650° C. their formation is rapid1. While it is possible to carry out laboratory roasts in such a way that less than 5 per cent of the total copper is present in the insoluble ferrite form, a closer temperature control is required than can readily be obtained in industrial furnaces. The flash" roasting effects and consequent high temperatures that occur as the calcine falls from hearth to hearth in the ordinary multiple-hearth roaster are probably largely responsible for the inevitable formation of some ferrites. The result is that in a commercial plant the extraction of copper would not average more than 90 per cent in a single 10 per cent H2SO4 leach. This is

Jan 1, 1937

By Frank Peterson

THE manufacture of gasoline by extraction or precipitation from the natural gases in which it is found, the present status of. the industry, its past development and future extensions; offer a subject which is so broad that to handle it in its entirety would require a voluminous paper. The writer will, therefore, attempt to concentrate the essential matter of the subject for a general presentation, giving some of the most interesting details of the factors that are important to the industry. This industry has drawn liberally on the principles of physics and chemistry, and, to a large extent, has had to adapt such information as is most useful-not from data recorded with reference to petroleum, but from data recorded with reference to general treatment of other materials. Because of the complex character of the petroleum series of hydro-carbons and the fact that data, such as solubilities, vapor pressures, etc., of the different petroleum compounds have not been determined, we are still working by rule of thumb in. some essential phases of the industry. Furthermore, the difficulties of determining such data are almost insurmountable. We have not one,, but two butanes to deal with-not one, but several, pentanes, hexanes, heptanes, and, as we ascend in the series the complexity and multiplication of isomers increases at such a rate as to make the task of isolating and studying their physical characteristics almost beyond the hope of possible attainment. The industry is the connecting link knitting the interests of oil producers and refiners into a much closer relationship than ever existed .prior to its inception and development. The relation between the producer and the refiner of petroleum prior to 1910 was. a rather antagonistic one in a commercial sense. It was to the interest of the producer of crude petroleum to sell it for a maximum consideration; the refiner's interest was to obtain the same product for a minimum consideration; therefore, each side of the business transaction retained within his own hands as far as possible the trade secrets of his business. Each side maintained an attitude of cold-blooded business sympathy only for the other. Cas-

Jan 12, 1917

By Reuben B. Ellestad, Fremont F. Clarke

In the early days of the lithium industry most of the production was from lepidolite, zinnwaldite, and amblygonite. Nearly all the early extraction processes described in the literature involve heating the finely ground mineral with sulphuric or hydrochloric acid. On subsequent water leaching most of the bases present in the mineral (especially aluminum) are dissolved as sulphates. As a result, the leach solution required extensive chemical purification before the lithium could be precipitated as carbonate. Following the remarkable growth of the lithium industry to its present size, zinnwaldite and amblygonite ores must be considered of minor importance only. Attention is now focused on spodumene, abundant enough in North America to be a major source of supply, and there are important supplies of lepidolite and petalite in Africa. The extraction processes described below all apply to spodumene, although several will also operate on other lithium minerals, such as petalite. Base Exchange with Alkali Sulphates: A distinct advance was made with the disclosures of Wadman and von Girsewalt. In these methods the finely ground silicate ore (spodumene or lepidolite) is intimately mixed with an excess of alkali sulphate (usually K2S04) in at least a 1 to 1 proportion, and the mixture was heated to a relatively high temperature. Base exchange results, with the formation of lithium sulphate. A water leach dissolves the lithium sulphate, together with the excess potassium sulphate. Successful operation of this type of process requires very thorough grinding and mixing, as well as careful temperature control. The use of K,SO, is objectionable from cost considerations since purification of lithium carbonate re- quires the use of potassium carbonate, if the K2S04 is to be recovered and recycled. The lower solubility of K,SO, as compared with Na,SO, is also objectionable, since it limits the concentration of the Li,SO, solution to be precipitated by K,CO,. Early laboratory-scale investigation of this process by Lithium Corp. was not encouraging

Nov 1, 1955

By K. Osseo-Asare

LIX63 In combination with DNNS selectively extracts nickel and/or cobalt from acidic leach liquors with pH values as low as 10 Nickel/cobalt and cobalt/nickel selectivities are achieved by varying the relative concentrations of LIX 63 and DNNS Increasing LIX63 concentration retards both extraction and stripping rates while DNNS has the opposite effect. Slope analyses of equilibrium data Indicate that both LIX63 and DNNS are present in the extracted complexes. Examples of possible flowsheets are presented.

Jan 1, 1981

By Colin Fink

TANTALUM and columbium occur together in tantalite and columbite ores, which may be considered as ferrotantalate (FeTa206), with part of the iron and tantalum replaced by manganese and columbium respectively, the general formula, therefore, becoming (Fe, Mn)O.(Ta, Cb)205. The ratio of tantalum to columbium is not fixed; the amount of tantalum may vary from one-third to three times that of columbium. Minerals having a high content of tantalum are called tantalite, while those possessing larger amounts of columbium are classified as columbite ores. These minerals are found in pegmatites and often occur in veins associated with cassiterite and wolframite, and may contain small amounts of tin, tungsten, titanium and silica.1

Jan 1, 1931

By C. A. Eligwe, F. W. DeVries, A. E. Torma

This study is an investigation on using hydrogen peroxide for tank-leaching of uranium with sulfuric acid. The optimum sulfuric acid concentration was found to be 0.03 mole 11 -'for a 25% pulp density suspension. The order of reaction with respect to sulfuric acid concentration was found to be ns0.75. The best results vith hydrogen peroxide were obtained at a 4.64 molar ratio of 6202 to U in the ore. The order of reaction was found to be zero with respect to hydrogen peroxide concentration. The theoretical maximum rate effect of Hz02 on uranium extraction was derived as Vm = 8.15 x mole &-'min-'. The highest rate experimentally attained was 8.09 x mole kL'min-'. It was found that the uranium extrac- tion was not affected by the pulp density up to the 50% used in this study. However, the final yieldswere significantly higher (over 90%) for leaches carried out in the presence of Hz02 than (less than 90%) for leaches carried out in the absence of H202. The reaction was found to follow a first order course with respect to substrate concentration (pulp density) regardless of the presence of H202. The effect of temperature was more explicit at moderate tempetatures (30 to 55 C) than at lower (10 C) or at higher (70 C) temperatures. At this latter temperature an almost complete extraction was realized even without H202. The apparent activation energies were found to be AEa = 2.68 kJ mole-' in the absence of H202, 0.5 kJ mole-'with Hz02 at 40 C to 70 C. and 4.72 kJ mole-' with Hz02 at 10 C to 40 C. All these activation energy values suggested that the uranium extraction process is diffusion controlled regardless of the presence of H202. Further, the change in activation energy in the presence of Hz02 indicates the possibility of change in the reaction mechanisms at lower and higher temperatures.

Jan 1, 1980

By R. Schuhmann, A. M. Gaudin, J. Dasher

Occurrrences of South African uranium have been known qualitatively for over twenty years, but no account was taken of them because of their low grade. In 1945, known uranium deposits were few, but their grades were 20 to 100 times higher than South African ores. Viewed in this light, the exploitation of South Africa's uranium is revolutionary indeed. Development of various analytical procedures capable of dealing with the needs of the project accounted for one-half of the cost and included: a) simple and automatic radiometric analytical procedures, b) sampling procedures appropriate to prevent sample contamination, c) procedures for sample and record-storing to accommodate many thousands of analyses per month, d) chemical methods giving high accuracy analyses for high grade samples not at radioactive equilibrium, and e) development of rapid procedures having moderate accuracy for low grade samples i.e., mill tailings and barren liquors. This task is continuing today with major improvements coming from time to time.

Aug 1, 1956

By James A. Barclay, Ralph C. Kirby

The US minerals posture will be increasingly dominated by three interrelated factors. First, when viewed over the long range, the US supply situation can be expected to steadily deteriorate as demand increases. Domestic high-grade ores have been used up, and other nations compete with the US for world supplies. Second, as environmental awareness becomes more acute, an aroused citizenry is demanding that minerals industries conform their operations to rigorous new standards. Finally, the changing energy situation that confronts the US is forcing an appraisal of energy-use patterns on operations previously guided solely by economic principles and not by national priorities. While future US mineral production and consumption patterns are unclear at this time, it is certain that US demand for minerals will continue to outrun domestic supply. Thus, the US is faced with a challenge of producing more minerals and metals from lower grade resources. Meeting this challenge means a strengthening of US research and development efforts, coupled with their application in the remaining leadtimes available. Some specific examples of how the US Bureau of Mines (USBM) is assisting in the processing of low-grade resources follow.

Jan 6, 1975

By S. W. Ross

In 1936 a description of the plant (Fig 1) and process employed by the Electrolytic Zinc Co. of Australasia Ltd. for the recovery of zinc from zinc concentrate by the electrolytic process was prepared. † During the twelve years which have elapsed since the preparation of the earlier paper, several major changes in the metallurgy of the process have been introduced. It is the purpose of the present paper to give a general description of these changes and thus to bring up to date the description of the plant and process. Summary The major changes in Risdon practice since 1936 have been: 1. Replacement of two stage roasting by a preliminary roast followed by the flotation of all the leach residue and the roasting of the flotation concentrate. 2. Screening of all calcine fed to the pachucas. 3. Continuous leaching of calcine and improved classification of pachuca discharge. 4. Close control of hydrogen ion concentration during purification for iron removal. 5. Recovery of cobalt as a good grade oxide. 6. Production of part of the zinc output in the form of "four nines" metal (99.99 pct purity). 7. Closer spacing of electrodes thus increasing the potential output of cathode zinc per cell by 50 pct. Changes which are in prospect and for which construction work is proceeding at the present time involve the starting up of: 1. Two suspension roasters. 2. A contact acid plant to produce 150 tons‡ of acid per day and replacing the existing Mills Packard chamber plant. 3. Extra power station capacity to permit greater current flow to existing cell room units. This will increase the output of cathode zinc from about 245 to 290 tons per day. Plans for the future envisage the building of an ammonium sulphate plant, the first unit of which will produce about 50,000 tons per year, and improved treatment of zinc plant residue for the recovery of zinc, lead and other metals. At the end of this paper tables of metallurgical data are presented relating to the year ending June 30, 1948. Details of Changed Practice Output In 1936 the production of cathode zinc amounted to about 200 tons per day. This has since been increased to about 245 tons per day while plant extensions are practically complete which will permit of an output of about 290 tons per day in the near future. Roasting Division ROASTING POLICY A major change has occurred in the roasting policy. Twelve years ago the method in use was to carry out a two stage roast in the first stage of which sulphide sulphur was reduced to about 6 pct. The pre-roast calcine was re-roasted in modified Leggo furnaces using coal as fuel, sulphide sulphur being reduced to about 0.8 pct. The whole procedure was described on pp. 482491 of the earlier paper. Although this roasting procedure had certain advantages it possessed some distinct disadvantages. For instance, it appeared uneconomical to heat up the entire input of pre-roast calcine to roasting temperature by the expenditure of fuel in order to oxidise a few percent of sulphide sulphur. It was argued that if the pre-roast calcine were leached and a process could be developed for the recovery of a zinc sulphide concentrate from the leach residue, this concentrate, small in weight compared with the pre-roost calcine, would probably roast autogenously, thus virtually eliminating the expenditure of fuel as well as greatly increasing the weight of sulphur oxidised per square foot of furnace hearth area. The obvious method of producing a suitable concentrate from leach residue was by flotation. It will be recalled (see p. 495 of the earlier paper) that when two-stage roasting was practised the leach residue was classified, the granular fraction was ground and floated while the slime fraction was thickened, filtered and dried ready for shipment to a lead smelter. This process worked quite successfully. However, when trials were made of leaching a calcine carrying several percent of sulphide sulphur the granular fraction still floated well, but the slime fraction carrying 8-10 pct sulphide sulphur yielded very poor results when subjected to flotation. This fact held up the application of "pre-roast" leaching for many years. However, successful flotation of the slime fraction of leach residue was finally achieved and in August 1940 the slime flotation plant began operation, while the leach-

Jan 1, 1950

By S. W. Ross

A. A. CENTER*—This paper reminds me of the beginning of the work of the Electrolytic Zinc Company of Australasia. Early work for this Company, as some of you may know, was done at the Bully Hill Plant in California. After working there for some time Herbert Gepp, now Sir Herbert, came to the Anaconda Co. plants in Montana where I met him. He spent some months there, in fact almost a year if I remember rightly. That was when we were breaking in the new electrolytic zinc plant at Great Falls, Montana. From there he went back to Australia and started in on the plant there. I believe they had an original plant of about 20 tons per day of cathode zinc. We heard from them for some time, until they were able to go along on their own, and they have done very well ever since as you have heard. Their practice, (the flow sheet, the leaching practice), has been quite different as reported in the paper and apparently they are still following that practice to some extent. While the earliest work on selective flotation was done down in Australia, the big companies there, strange to say, were far behind the American companies in taking it up; and it is only in comparatively recent years they have gone to the alkaline circuit and dropped out thereby more of their iron and lead. The zinc plant now is up to a capacity of 100,000 tons a year and I believe that may be notched up to about 105,000. T. H. WELDON*—I would like to ask

Jan 1, 1950

By G. H. Anderson

Cadmium-coppeR precipitate, a byproduct of the purification stage of the zinc plant, is composed mainly of zinc, cadmium and copper in varying amounts depending on the efficiency of precipitation and the cadmium and copper contents of the impure solution treated. The composition range is approximately: cadmium 10-12 pct, copper 6-8 pct, and zinc 3&35 pct. As received at the cadmium plant, the precipitate is a dark gray to black press cake produced by filter pressing the flocculent cadmium-copper precipitate formed when impure zinc solution is agitated with zinc dust. The details of the cadmium-copper precipitation are to be found in the paper "Electrolytic Zinc at Risdon, Tasmania," by W. C. Snow. Transactions AIME, 121, 501. The treatment, in addition to recovering cadmium as metal, yields a copper product as a residue for realization and recovers in solution for return to the zinc plant, the excess of zinc dust used during purification. The recovery of cadmium metal is approximately 200 tons† per year, but, with the amount of copper residue recovered, varies with the zinc production tonnage, composition of the original concentrates, degree of roasting and other operational factors. The operations involved in the recovery of the foregoing materials are carried out in a building adjacent to the purification section of the zinc plant and can best be described by dividing the process into the following stages: 1. Oxidation and Grinding of the cadmium-copper precipitate. 2. Leaching and Filtering. 3. Precipitation of cadmium. 4. Oxidation and Grinding of the precipitated cadmium. 5. Leaching oxidized cadmium precipitate and Purification of leach solution. 6. Electrolysis. 7. Melting, Casting and Packing. A feature of the process is the use of two distinct solution circuits. Spent electrolyte from the zinc plant circuit containing about 10 pct sulphuric acid is used as the primary solvent of the cadmium and zinc present in the oxidized precipitate. When the cadmium is later separated by precipitation and filtering, the filtrate, originally zinc plant spent electrolyte and now fortified in zinc, is returned to the zinc plant. The precipitated cadmium, after oxidation, is redissolved in spent electrolyte from cadmium electrolysis which solution is in closed circuit within the cadmium plant except for discards to the zinc plant circuit as mentioned in Section 5 hereinafter. (Fig 1.) Details of the various operations follow. I. Oxidation and Grinding of the Cadminm-copper Precipitate The precipitate having had a preliminary drying by compressed air in Dehne filter presses in the zinc plant is trucked to a storage platform of sufiicient length to store 3 to 4 days' production separately. After 48 hr exposure to atmosphere, oxidation is sufficient to enable all cadmium and zinc but only a portion of the copper to be dissolved in dilute sulphuric acid. The oxidized precipitate is shovelled into trucks and, after weighing and sampling, is broken in size by means of

Jan 1, 1950

By G. H. Anderson

H. R. HANLEY*—I have been asked to discuss briefly the development of rotating cathodes for the electrolytic deposition of cadmium. The earliest recorded use of rotating cathodes was by Hoepfner at Frufurt, Germany about sixty years ago. He elec-trolized zinc chloride solution using diaphragms to separate electrodes. In the early experimental work of the Bully Hill Copper Mining and Smelting Co., Shasta County, Calif., rotating aluminum cathodes 4 ft in diam were used in the electrolysis of an acid zinc sulphate solution. Finished cathodes weighing up to 400 lb were produced. Because of mechanical difficulties, this type of cathode was abandoned for zinc, but was later used for cadmium because of the relative smoothness of deposit in comparison with stationary plates with comparable current densities. Cadmium sponge which forms on the cathode at moderate current densities (without special treatment) is entirely eliminated by a slow rotation. The rate of rotation of the cathode has an effect on the mechanical nature of the deposit. A high rate of rotation concentrates the adhering electrolyte on the shaft; a moderate rate appears to concentrate on the cathode a short distance out from the shaft tending to corrode the deposit in the form of a ring. At a very slow rotation (2 to 3 rpm) the adhering electrolyte gravitates nearly vertically, thus avoiding the cutting ring referred to above. The true explanation for the smoother deposits obtained on rotating cathodes may not be given definitely as the numerous factors involved are not thoroughly understood. Smooth deposits are obtained when the orderly growth of the metal crystals in the cathode lattice are disorganized. Thus the crystals form and grow for a very short interval when they are arrested and a new crystal forms. The continued growth of the original crystals provides large crystals and a rough deposit. Also if the acidity of the electrolyte is low, hydrogen gas bubbles adhere to the deposit. As the cathode is rotated the gas surface is brought into the atmosphere where they burst; thus the deposit is made on a surface relatively gas-free. An aluminum hub distance piece was riveted to each aluminum disk 4 ft in diam, slipped on a 4 1/2 in. steel shaft and pressed tight to prevent acid electrolyte seeping through to the shaft. The 9-cathode assembly was supported on insulated bearings. Electrical contact to the shaft was made through what was equivalent to a copper pulley. Sufficiently high conductivity brushes were placed on the face of the pulley to lead the current to the cathode bus bar. The assembly was driven by a link belt contacting a sprocket insulated from the shaft. The lead anodes were semicircular and supported on porcelain insulators placed on the bottom of the cell. Two anodes were provided for each cathode to permit an 8-in. space between them without increasing the ohmic resistance. This ample spacing permitted easy stripping of deposit with the assembly in place. Cathode cadmium was melted under 650 W cylinder oil. After casting, the primary slabs were remelted under molten caustic soda and cast into pencils 1 1/32 in. in diam. Rotating cathodes for deposition of cadmium are used at Risdon, Tasmania, and at Magdeburg, Germany. W. G. WOOLF*—This paper is very-interesting to me because in our work at the Electrolytic Zinc Plant of the Sullivan Mining Co. we had an exactly similar problem—that is, a method of producing cadmium from our purification residue, the recovery of the contained copper as a copper precipitate which could be sent to a copper smelter and the production of merchantable cadmium. It is interesting to me, not knowing of the work of the Risdon people, how closely we approximate them in their main metallurgy, diverging at several interesting steps which I would like to discuss for just a moment. For example, at Risdon they oxidize their purification residue. In our practice we take the current residue as it is produced in the purification department of the zinc plant and process it in the cadmium plant. The only oxidation that it obtains is the oxidation in the presses, the dumping of the presses and the collection and transportation of the residue to the cadmium plant. We find that the leaching of that residue does not necessarily require the oxidation step that the Risdon people evidently find necessary. The discussion of oxidation comes in again in the matter of the treatment of the precipitated cadmium sponge with zinc dust which again at Risdon is oxidized but which we do not attempt to oxidize except as it oxidizes itself in the storage. There is a partial oxidation which cannot be avoided, as Mr. David-sou pointed out, but we make no attempt to attain a complete oxidation and we dissolve the cadmium sponge in the sul-

Jan 1, 1950

Established as a Division November 17, 1948 T D Jones, Chairman O C Ralston, Past Chairman R R. McNaughton, Chairman-elect B. W Gonser '53, Vice-Chairman P. T. Stroup '54, Vice-Chairman Ernest Kirkendall, Secretary 29 West 39th Street, New York City

Jan 1, 1952

Established as a Division November 17, 1948 B W Gonser, Chairman J C Kinnear, Jr, Past Chairman H H Kellogg, Chairman-Elect R C Cole, Vice-Chairman, '58 A E Lee, Jr, Vice-Chairman, '59 W R Opie, Vice-Chairman, '60 R W Shearman, Secretary AIME, 29 West 39th Street New York 18, N Y

Jan 1, 1957

By W. R. Opie, O. W. Mole

By confining the electrolytic reduction of TiCl4 to the interior of a porous basket-cathode the electrolyte between the anode and the cathode can be kept free of reduced chlorides of titanium eliminating undesirable reactions of reduced titanium chlorides with brickwork or oxygen in the cell atmosphere. Semiwalls are not needed. Operating conditions are given and discussed. Titanium yields based on TiCl4 introduced are 93 pct. Cell voltage and amperage characteristics are adaptable to multiple cathode-series cell urmngements. EXPERIMENTS conducted in the National Lead Co., Titanium Division, Research Laboratories showed that titanium metal could be deposited in an electrolytic cell in which titanium tetrachloride was introduced through a tubular cathode.' The reduced chlorides as formed were confined to the vicinity of the cathode. They were reduced to form a cocoon-shaped growth of sponge titanium metal at the end of the cathodic tube below the surface of a sodium chloride-strontium chloride electrolyte. No diaphragm was needed.' Although high-purity, coarse crystalline metal was produced in the cocoon growth, the yields of metal removed from the cell, based on the amount of titanium introduced as TiCl4, were usually only 40 to 60 pct. The growth of the cocoon deposits was away from the cathodic tube for introduction of TiC14 toward the anode following the flu lines. The reduced chlorides of titanium diffused through the deposit and were reduced to titanium electrolytically within the deposit or on the outer surfaces. Deposition within the pores of the cocoon was detrimental to further deposition because it plugged the passages used by the reduced chlorides to diffuse away from the point of titanium introduction. As plugging due to deposition in the pores proceeded, the reduced chlorides in the center of the cocoon would force their way out by forming a channel and would escape from the vicinity of the cathode without being reduced to metal. Some work had been done previously1, 2 which indicated that if the end of the cathodic tube for introducing TiC14 was surrounded by a screen connected to the tube so that it too was cathodic, growth could be made to occur within the screen. Direction of growth was observed to be from the screen toward the point of TiCl4 introduction. Through a series of design modifications a cathode evolved which consisted of an introduction tube surrounded by a perforated metal basket as shown in Fig. 1. Modifications of this design are described in Refs. 3, 4, and 5. This basic cathode designa" was incorporated in electrolytic cells containing graphite anodes and constructed of high-silica brick refractory for containing the electrolyte (see Fig. 2). The inner crucible was surrounded by insulating brick and the entire unit contained in a welded steel shell. Suitable cooling chambers with inert gas atmospheres were devised so that the cathode could be removed from the cell without exposing the deposit to air while hot. Various alkali and alkaline earth chlorides were used as electrolytes.

Jan 1, 1961