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By N. Melnyk, H W. Habgood

The conventional low temperature process for extracting' helium from natural gas involves liquefying the whole gas stream in order to remove the relatively small fraction of helium. A process based on the selective diffusion of helium through a semi-permeable barrier is, in principle, more economical and flexible, particularly for the treatment of small re-serves and low concentrations. The well-known permeability of glass to helium offers the possibility of such a diffusion process and McAfee of the Bell telephone Laboratories showed in 1958 that practical separations could be achieved by passing natural gas over bundles of fine capillary glass tubing. Developmental studies have been carried out involving larger units and more extended field tests than those of McAfee. Fine capillary tubing of Pyrex glass 0.0035 in. diameter was prepared by drawing ordinary 6 mm. laboratory tubing in a furnace. Extraction units were pre-pared containing about 10,000 such tubes, 4 ft. long and cemented inside

Jan 1, 1961

By Jafar Safarian

Bauxite is the main raw material used for the production of alumina (Al2O3) through the well-known commercial Bayer process. This process has significant challenges such as limitation in using low-grade bauxites as they contain significant amounts of impurities such as Fe, Si, Ti. The Bayer process residue, which is known as red mud, is also a global environmental challenge due to huge amount of this low value residue production. An alternative sustainable process with high potential to solve these problems and produce valuable and consumable by-products is a pyrometallurgical-hydrometallurgical process in which the low-grade bauxite ore is treated through a smelting-reduction process, yielding iron alloys and a calcium-aluminate slag. Alumina is then produced from the slag by hydrometallurgical treatment. In the present work, the reduction of pellets produced from different bauxite ores by hydrogen is studied and it is shown that complete iron oxides reduction is possible. Further smelting and smelting-aluminothermic reduction of the reduced pellets show that iron and silicon ferroalloys can be produced, in addition to a proper slag for alumina extraction.

By S. M. C. Santos

Preliminary bench-scale studies were carried out on the leaching of a zinc sulphide concentrate from Somincor, Portugal, and the purification of the resulting pregnant solution using solvent extraction techniques. The sulphide concentrate contained 36% Zn, 36% S, 2% Fe and 4% Cu. The leaching was carried out with sulphuric acid in the presence of ferric sulphate as the oxidant. Important leaching parameters, such as the effect of reaction time, the solid-liquid ratio, temperature and concentrations of acid and oxidant, were investigated. After leaching, the recovered solution was contacted with an organic phase containing Acorga 5640 to remove the copper. Subsequently, the removal of iron from the leaching solution was achieved with a mixture of Cyanex 272 and TBP. This solvent mixture was relatively selective for iron over zinc. The stripping of the loaded solvent was performed with 200 g/L H2SO4. Six countercurrent extraction stages achieved a separation of about 99% of the iron from the leaching solution. The iron-free leachate can be further treated to recover minor metals by cementation, and finally, zinc by liquid-liquid extraction. The advantages of the suggested process relative to the traditional jarosite process are discussed.

Jan 1, 2006

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 1.0. Nickel/cobalt and cobalt/nickel selectivities are achieved by varying the relative concentrations of LIX63 and DNNS. Increasing LIX63 concentration retards both extraction and strip-ping 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, 1978

By M. J. Steffens

ESPLIM is a novel separation technique that combines the advantages of solvent extraction and electrostatic dispersion but its application in the extraction of nickel by the direct solvent extraction route and the effect of high electrostatic field on the stability of organics have not been explored. These were investigated in this study and it was found that the technique allows 97% extraction of the nickel in a single stage compared with 3 stages by the conventional solvent extraction. Also, three months of exposure to 5.0 kV under simulated operational conditions had no adverse effect on the stability of organics.

Jan 1, 2005

By Ting An Zhang, Chengzhi Jiang, Xiujing Zhai, Feng Xie

The extraction and concentration of nickel from aqueous solutions by emulsion liquid membranes (ELMs) using tributylphosphate (TBP) as extractant has been investigated in this research. The emulsion liquid membrane consists of a diluent (kerosene), a surfactant (Span 80), a mobile carrier (TBP), and a stripping solution (ammonia solutions). Important factors influencing the separation process including membrane composition, feed composition, and mixing speed have been examined. The results show that more than 90% of nickel in the feed solution could be extracted by ELMs under the experimental conditions, indicating the feasibility to use the designated ELMs to detoxify nickel-containing industrial waste solutions.

Jan 1, 2014

By Z. H. Khan, A. K. Saha, D. D. Akerkar

The possibility of extracting nickel from a low-iron, highly siliceous nickel ore of Indian origin using roast reduction followed by an ammonia leaching process has been examined. The ore used in the investigation contained 0.82 wt% Ni, 6.20 wt% Fe3O4, 12.04 wt% MgO and 60 wt% SiO2. Phase changes in the constituent minerals on heating were studied by differential thermal analysis which revealed endothermic peaks at 110 and 695 degrees C and an exothermic peak at 810 degrees C. Significant process variables in studies of roast reduction include the amount of reductant, the temperature of reduction and chemical kinetics. Maximum nickel extraction was achieved by reducing the ore with 10 wt% fuel oil at 750 degrees C. The reduced ore was given a preconditioning treatment in concentrated ammonium hydroxide solution to oxidise most of the metallic iron and was then leached in aqueous ammoniacal solution at ambient temperature to dissolve nickel. This gives 88.5% extraction of nickel as soluble ammine complexes.

Jan 4, 1992

By Vladimir Lobanov, Vladimir Skorohodov, Andrew Evdokimov, Ural State Technical University 19, Boris Radionov

"The bulk of raw materials in metallurgy of secondary platinum metals are the wastes such as multilayered ceramic-metal systems, e.g. the spent catalysts of the chemical and petrochemical industry, automobile catalysts, etc. Due high chemical resistance of a ceramic basis the extraction of platinum metals by leaching even at very fine crushing is poor. The study of sorption leaching of platinum and a palladium from the spent automobile catalysts are carried out. The average content of PGM is 0.5%. A few methods of raw materials sampling were compared: 1) direct hydrometallurgical leaching of platinum metals from the fine-grained catalyst and atomic absorption analysis of the obtained solutions; 2) fusion to a metal or sulphidic collector of precious metals with the alloy analysis by direct spectrometry; 3) fusion with dissolution of a precious metals collector and atomic absorption analysis of PGM in solutions. Leaching allows detecting out no more than 90% of a palladium and 80% of platinum. Fusion to a collector gives the best results at the chemical ending. Researches on sorption leaching are executed. Under optimum conditions the extraction of platinum metals to concentrates is comparable with similar indicators of collector fusion.The large part of raw materials in metallurgy of secondary platinum metals are the multilayered or tridimensional ceramic-metal systems, in particular the spent catalysts of the chemical and petrochemical industry, automobile catalysts, ceramic-metal condensers, etc. The content of the sum of PGMs can be from hundreds grams per ton to several percent. For processing of such materials the hydrometallurgical methods of platinum metals leaching by various reagents are used commonly. High chemical resistance of the ceramic basis covering the metal particles causes low recovery even at very fine grinding. Other fundamentally different method of catalysts opening includes dissolution of the ceramic basis in the solutions of hydrofluoric acid and the subsequent recovery of platinum metals from insoluble residue. Application of this method is associated to use of corrosive medias and appropriate equipment. Fusion of the specified materials with collecting of PGM by copper, nickel or lead at the specialized enterprises provides higher extraction in semiproduct. At the same time, complexity and duration of the subsequent extraction of platinum metals concentrates causes high total cost per unit. Thereby this method is economically acceptable only for rather poor raw materials (no more than 0,1%). Undoubtedly, that the raw materials with the high content of PGM are reasonable to process by individual technology. In the present work the processing of some kinds of ceramic-metal raw materials, particularly automobile catalysts (neutralizers) with various collectors at the conditions of a target fusion are investigated."

Jan 1, 2008

By R. J. Traill

Introduction Following the discovery of high-grade deposits of pitchblende in the Great Bear Lake area of the Northwest Territories by Mr. Gilbert LaBine in May, 1930, samples were submitted to the Mines Branch for examination and investigation as to suitable methods of treatment (1). The purpose of this paper is to present, briefly, the results of the investigative work conducted on the ores and an outline of the methods developed for the extraction of the radium content and recovery of the by-products. The paper is presented in two parts. Part I gives a review of the history of radium production and of the principal processes used in other countries. Part II describes the work and gives the results of the Mines Branch investigation. Part 1-Radium Production In Other Countries Historical Outline Uranium was discovered in 1789, and more than a century later Madame Curie, while studying the physical properties of this element, observed that the ore of uranium exhibited greater activity than the pure uranium com-pounds she had prepared and traced the cause to the presence of a new element which she named radium. Eventually, research proved radium to be a disintegration product of uranium, and always present in uranium ores.

Jan 1, 1933

By M. Tanaka, H. Narita, T. Fuchikami, K. Morisaku, K. Nagao, T. Yoshida, K. Kuroda

The effect of various N-substituents on the performance of amide-containing tertiary amine compounds in the extraction of Rh(III) from HCl solutions was investigated to optimize the structure of these compounds for industrial use. It was found that N-2-ethylhexyl-bis(N-di-2-ethylhexyl-ethylamide)amine and tris(N-di-2-ethylhexyl-ethylamide)amine, which have long, branched alkyl chains, were suitable for Rh extraction, because they were soluble in a practical diluent (80 vol% n-dodecane?20 vol% 2-ethylhexanol) and stable against highly concentrated HCl/Rh solutions, and showed high selectivity for Rh(III) over Pd(II) and Pt(IV).

Jan 1, 2014

By James R. Evans

Orange County, adjacent to the populous and industrialized Los Angeles area, is the fastest growing county in California and is second only to Los Angeles County in total population (figure 1). In addition to an equable climate and a burgeoning economy, there is room in Orange County for growth and expansion. Growth over the past decade has resulted in rapid development of industrial tracts, housing areas, and shopping and commercial centers, mostly in former agricultural areas. The value of new building in 1972 was a record amount-over I billion dollars (figure 2). Problems relating to the proper direction of growth are the concern of both government and the private sector. The intelligent and efficient use of areas to be developed requires planning for the conservation and protection of the County's natural beauty and for the orderly development of natural resources. The availability of sand and gravel, which is used in many phases of construction, will be a major controlling factor in the future of the County.

Jan 1, 1974

By J. P. Hager

The formation of the vapor complex AgFeC14 (g) baa been identified and its thermodynamic properties determined. The vapor pressure of silver chloride can be enhanced by a factor of 15-20 due to the formation of the vapor complex. The vapor pressure of both AgCl (g) and AgFeC14(g) were measured using a double-zone transpiration .technique. Gibbs free energies have been determined for the vapor transport reactions. Laboratory kiln tests were conducted to confirm the enhanced recovery of silver through the formation of the AgFeC14(g) vapor complex and to indicate the opportunities for process development using this new vaporization chemistry.

Jan 1, 1985

By Urs Peuker, Thomas Mütze, Thomas Leißner, Inga Osbahr

"Mining in the Ore Mountains (Germany) has taken place for hundreds of years and in several stages. Each stage produced its typical tailing. According to the former state of the art of the processing much valuables could not be extracted. This was caused by complex interlocking of the minerals, low grades, or by upgrading processes not sensitive enough for small particle sizes. Thus the processing of these fractions was uneconomically. Modern technical possibilities and rising metal prices bring these tailings disposals into focus for the processing of strategic metals. Mining disposals can be classified in heaps with coarse, low grade rock, which did not undergo a processing, slags and fly ash from smelting, and tailing disposals from mineral processing. The latter is under investigation to integrate them into a geographic information system. The mineral processing of the material will be part of the database besides information about geographic location, structure, amount of valuables, and details of ownership of the heap. The tailings disposals are composed of coarse, low grade, interlocked particles from density separation processes, medium size particles, which are tailings from flotation, and fines with liberated valuables, which did not undergo flotation. Therefore mineral processing of these disposals comprises the separation of liberated gangue by classification, beneficiation of locked valuables with density separation, liberation of valuables by grinding, and beneficiation of liberated valuables with flotation. The presented work shows the results concerning the composition of one exemplary heap and results of the classification as well as of the preconcentration tests achieved with material from this heap."

Jan 1, 2014

By Hassan Saalman, Mahmoud Mahmoud, Omneya El Hussaini

The Ferruginous sandstone ore was obtained from Ramlet Hemeyir area, Southwestern Sinai, Egypt, was found to contain 10% rare earth elements (REE). A representative sample has been subjected to sulfuric acid agitation leaching. About 93% of the REE content was released by mixing the ground sample to -100 mesh with concentrated H2SO4 at solid/liquid (S/L) ratio of 1/2 for 5h at a temperature ranged from 250 to 300o C. The REE was precipitated from the prepared sulfate leach liquor of pH 1.0 by adding 35% oxalic acid at 25o C. The precipitation yielded 98% REE. For selective separation of yttrium, the rare earth cake was leached with 31.5% nitric acid. Next, the aqueous solution was contacted with di-(2-ethylhexyl) phosphoric acid (D2EHPA) where 98% yttrium extraction was achieved. Stripping was done with hot H2O (80o C). Finally, a precipitation with oxalic acid was done followed by ignition at 950o C. A yield of 95% yttrium oxide was produced.

Jan 1, 2014

By Hsing Kuang Lin

Extraction of zinc from chloride solution with dibutyl butylphosphonate (DBBP) in Escaid 110 has been investigated. The distribution coefficient of zinc was found to be independent of equilibrium pH. This independence indicates that the mechanism of the extraction may be solvation. Slope analysis for the system of dilute zinc chloride solution reveals that two moles of DBBP react with one mole of zinc. A series of tests were conducted to bring DBBP to its full loading capacity and the analysis of the results confirms this stoichiometric factor of 2. Extraction isotherms were established by varying either the AIO ratio or the concentration of zinc in the aqueous feed. Both curves were found to be identical.

Jan 1, 1990

By B Harvey

Achieving community and stakeholder endorsement during life-of-mine planning and implementation requires a business-connected approach, as opposed to charitable giving, disconnected offsets and environmental adventurism.CITATION:Harvey, B, 2014. Extractive companies, development and environmental agendas, in Proceedings Life-of-Mine 2014 , pp 19–22 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Jul 16, 2014

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

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

By R. G. Ward, A. E. El-Mehairy

A technique was developed to calculate the density of liquid metals from the profile of a weighed levitated drop obtained by emitted light photography and calibration. The density of liquid copper was determined over the temperature range 1370" to 2100°K and expressed with the equation: The molar volumes and thermal coefficients of expansion are calculated. Copper, upon melting, was found to expand 3.34 pct. A knowledge of the density of liquid metals is essential as it is a parameter appearing in most theories of the liquid state. The liquid density is also necessary for the calculation of the commercially important contraction occurring on solidification. Unfortunately good density values are rarely available and the present work was undertaken to establish a new method of density determination free from the limitations of the existing methods. For liquid metals with high melting points, the variation and the limited number of density values reported in the literature have been caused primarily by difficulties in technique, a matter which has been adequately discussed by Urbain.' In all the methods used for measuring the density of the high-melting liquid metals there are sources of error, and corrections have to be made. For example, in the method of balanced columns, the formation of gas bubbles in one or both arms was a great source of error. In the pyknometer3 and immersed-sinker methods, corrections of certain volumes for thermal expansion to the operating temperature exceed 4 pct. In the maximum-bubble method5 a correction for the thermal expansion of the bubble-tube is used (about 1.6 pct); a second correction takes into account the change in the volume of liquid displaced by the bubble-tube (about 3.5 pct). Another method used is based on the shape of a drop of liquid, at rest on an inert refractory plaque, obtained photographically or radiographi-cally. The volume is calculated from the shape, which is sensitive to the surface tension and supporting material, by some intricate empirical relation. The drop contour changes with 90 deg rotation of the support.7 The application of all methods is limited by reaction between liquid metal and the apparatus. The successful stabilization of a mass of liquid metal during levitation melting8 afforded a technique for measuring the density of liquid metals out of contact with solid materials. The technique was developed by using copper as the density of liquid copper has already been studied extensively, thus allowing comparison with the new method. It consists of calculating the volume from the dimensioned profile of the levitated drop obtained by emitted-light photography and careful calibration. The molten egg-shaped drop spins around the magnetic axis of the coil (lined vertically) at a speed which seems to increase with increasing temperature. The method does not involve corrections and the experimental setup allows the use of vacuum or special atmospheres. The maximum operating temperature is limited by excessive evaporation of metal from the droplet. EXPERIMENTAL Levitating System. A stabilizing ring was used in conjunction with a 3-turn levitating coil energized by a 450-kc per sec, 10-kw Toccotron with a high current-low voltage output stabilized to f 1 pet.' APyrex glass tube with a Pyrex Optical flat window inserted through the coil and ring allowed the use of special atmospheres during levitation melting, as shown in Fig. 1. Optical System. Fig. 1 shows the optical arrangement used to photograph the profiles of the drop, parallel and perpendicular to the vertical spinning axis, simultaneously on the same frame of a high-speed 35-mm film. The optical system was adjusted to avoid any distortion of the profiles and to ensure that both profiles are in focus. The length of path from object to objective was about 30 cm, and a magnification factor close to 1 was obtained with the single-lens reflex-camera system. Temperature Measurement and Control. In operation, the specimen temperature was constant to 5 C for a fixed power input to the levitating coil and fixed rate of gas flow through the tube. The temperature was measured by an automatic two-color pyrometer (Coloratio) checked at the melting

Jan 1, 1963

By P. W. Bennett, E. M. Elkin

A new technique for the recovery of palladium and platinum and sludge from go12 electrolyte eliminates many of the drawbacks of the zinc-dust cementation process. In the electrolytic refining of gold by the Wohwill method, the electrolyte contains about 100 gpl gold as AuCl, and 100 gpl free hydrochloric acid. Any palladium and platinum contained in impure gold dissolve and accumulate in the electrolyte. When their concentration approaches that of gold, it becomes desirable to discard the electrolyte and to recover the gold and the palladium and platinum. As practiced at Canadian Copper Refiners until recently, discarded electrolyte was treated with sulfur dioxide to precipitate the gold. 2AuCl3 + 6H2O + 3SO2 —2Au + 6HC1 + 3H2SO4 The gold precipitate was filtered off, washed with water, and melted with scrap anodes. The wash water was added to the gold-free filtrate and treated with zinc dust to cement the palladium and platinum. PdCl2 + Zn — Pd + ZnCl2 PtCl4 + 2Zn—Pt + 2ZnCl2 The precipitate was separated and sold as Pd-Pt concentrate, and the barren filtrate and wash water were discarded. The receipts of palladium and platinum at this company were too small to warrant their refining. The process suffered from a number of disadvantages. Handling the gold-free solution was disagreeable, as it was laden with sulfur dioxide even after blowing with air overnight. Subsequent treatment with zinc dust was also troublesome. A large excess of zinc dust was required. Spray, acid mist, and vigorous evolution of hydrogen accompanied the reaction. The Pd-Pt precipitate was grossly contaminated with occluded unreacted zinc and with yellow granules of sulfur, thought to be formed by the reduction of sulfur dioxide and its derivatives. Repeated boiling of the precipitate with hydrochloric acid and washing with water decreased somewhat, but did not eliminate, the zinc. After drying overnight, the precipitate hardened to a clinkerlike mass that was difficult to grind. Grinding, handling, and packing created heavy dusting. Even weighing in an analytical balance generated dust, indicating that the powder was easily charged with static electricity. The total palladium and platinum content of the powder varied from 56 to 72 pct, with an average of 65 pct. The powder dissolved in aqua regia with difficulty, leaving a small amount of insoluble residue. However, the main drawback of the process was the strongly hygroscopic Pd-Pt product. The powder showed a marked though erratic increase in weight and a corresponding decrease in assay on exposure to air, even during the course of laboratory analysis. Such changes were the source of disagreement between Canadian Copper Refiners and the buyers of concentrate. The cause of the change in weight is believed to be hydrogen, liberated by the action of zinc dust on hydrochloric acid. Some of this hydrogen was adsorbed so strongly by the precipitate that it could not be driven off during the drying. On exposure to air it oxidized catalytically, forming water. Experiments soon showed that the entire process of treatment of discarded electrolyte then in use would have to be changed. A small quantity of apparatus was moved into the gold room, and experimentation was held to a minimum compatible with the development of a new process. PALLADIUM AND PLATINUM PRECIPITATION It was thought that zinc could be replaced with a reagent other than a hydrogen-evolving metal. Semiquantitative experiments showed that platinum and palladium could be precipitated completely from the gold-free solutions with such well-known reagents as sodium formate, formic acid, formaldehyde, and paraformaldehyde. Sodium formate was the preferred reagent, since the other three are volatile and somewhat toxic. The gold-free solutions used were those saturated with sulfur dioxide, partly freed of sulfur dioxide by aerating overnight, completely freed by boiling, as well as strongly and weakly acidic, neutral, and alkaline solutions. The reactions are complex and can be represented by these over-all equations: PdC1, + HCOONa — Pd + NaCl + HC1 + Co2 PtCl4 + 2HCOONa — Pt + 2NaCl + 2HC1 + 2CCX, Strongly acidic solutions required as much as five times the theoretical amount of sodium formate as did solutions neutralized to pH 4.5. Increasing the pH decreased the consumption of

Jan 1, 1965