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By Takafumi Kondo, Satoshi Yamashita, Noboru Masuko

"Aqueous oxidation of phosphite ions to phosphate ions with dissolved oxygen was examined at 80° C and pH 4.5 mainly from the stichiometric point of view. Dissolved oxygen alone can not oxidize sodilim phosphite in aqueous solution, but when sulfur dioxide is coexistent, cooperative oxidation for both sulfite and phosphite can occur in aqueous solution. Sulfur dioxide itself is well known as a reducing agent, but it also reacts as an oxidation-promoting agent for other species under a certain condition. So sulfur dioxide is· a promising cheap reagent for waste phosphite processing.IntroductionIn a liquid-phase oxidation reaction using the dissolved oxygen gas, the eoexistence of a copper salt is required generally. Recently, it was reported that the oxidation reaction progressed by using mixed gas of sulfur dioxide and oxygen without the copper catalysis, and the attention has been collected1·3). The present authors also noticed the phenomenon since the early time and have been studying on the reaction mechanism of sulfur dioxide in liquid phase oxidation 4l. It was found that; by using the SO2-O2 mixed gas, the oxidation of phosphite ions to phosphate ions proceeded efficiently in sulfuric acid solutions. In the present report, the applicability of SO2-O2 mixed gas as a cheap oxidizing agent to the industrial processing of the waste solution of electroless nickel· plating is investigated. It is well known that the sulfur oxide dissolved in aqueous solution is oxidized ·by the oxygen in the air to sulfuric acid according to the following equation"

Jan 1, 2000

By M Phil Schwarz

"A CFD model for the gas-side of an impinging jet iron bath reactor has been developed to assist in the interpretation and design of oxidizing gas-melt reaction rate experiments. Heat transfer and reaction at the surface have been included. A free surface model, which solves for the liquid motion within the bath as well as the gas motion above the bath, has also been developed. This model also predicts extent and shape of the dimple formed on the liquid surface by the impinging jet. Both models have been run for conditions typical of jet impingement experiments using CO2 , H2O and O2• The main conclusions are• Results from the model for gas-side mass transport are in good agreement with the empirical correlation of Belton and Belton (1980)• Experimentally determined rates of decarburization by CO2 should be corrected for mass transfer because the experiments are often carried out under mixed rate control, eg for gas flow rate 10 L/min when the sulphur concentration is lower than 0.045• If the rate constant for oxygen reaction is greater than about 5 mol/m2.s.atm, it cannot be determined using a gas flow rate of 10 L/min or lower because of mass transfer control.• A cavity of depth 4.5 mm is predicted for a gas flow rate of 10 L/min and this substantially changes the flow field (and hence reaction rate) compared with a simulation in which the surface is assumed to be flat."

Jan 1, 1999

By F. Patisson

One of the major issues with multiparticle reactors is to handle their multiscale aspect. For modeling, it usually comes to coupling a reactor model (describing the phenomena at the macroscopic scale) with a so-called grain model (simulating the behavior of a single grain or a particle). An interesting approach proposed by H.Y. Sohn (1978) is to use the law of additive reaction times in order to calculate, approximately but analytically, the reaction rate of a particle in the reactor model. Its great advantage, compared to a numerical grain model, is to drastically reduce the computation time, particularly in the case of complex reactor models. This is the approach we retained for modeling the moving bed furnace, a counter-current gas-solid reactor used in the nuclear fuel-making route for producing uranium tetrafluoride from uranium trioxide. The numerical model we developed is 2-dimensional, steady-state and based on the finite volume method. It describes solid and gas flow, convective, conductive and radiative heat transfers, and six chemical reactions involved in the process. The law of additive reaction times is used to calculate analytically the rate of the three principal gas-solid reactions at every discrete point in the reactor. We have demonstrated the validity of this approach by comparing its results with those calculated from a numerical grain model. Also detailed in the paper are the main results of the moving bed furnace model itself and the possibilities of optimizing the process revealed by the calculations.

Jan 1, 2006

By M. A. Gimenes

The utilization of chlorination in extractive metallurgy and advanced ceramics areas has been widely investigated as a preparative route in order to obtain intermetallic compounds, which are used as precursors in the development of new materials and process. The major processes of decomposition of rare-earth ores use sulfuric acid and sodium hydroxide at high temperatures, however there is not much work concerning chlorination. In this work, a systematic study of the reaction between xenotime (REPO4), chlorine and carbon has been performed. Particular emphasis was on kinetic studies to establish optimized conditions for the reaction. The kinetics of chlorination of xenotime raw material by rare-earth elements/compounds has been studied over a temperature range from 600°C to 950°C. The influence on the rate of conversion of xenotime to RECl3 on temperature, partial pressure of chlorine, carbon content, and particle size were investigated. A global rate equation that includes these parameters has been developed. The results show that the process follows the unreacted core-shrinking model with a formation of a porous product layer. The powder X ray-diffraction technique corroborated this model showing clearly the patterns related to the formation of yttrium oxychloride (YOCl), indicating that the reaction mechanism involves the presence ofan intermediate step before the formation of lanthanide chloride.

Jan 1, 2000

By Aly M. Abdel-Rehim

The present work deals with a study of the mechanical activation of processing of Egyptian monazite by its simultaneous ball-milling and pressure leaching in order to improve the recovery of thorium and lanthanides from monazite. Experiments of simultaneous ball-milling and alkaline leaching of monazite contrary to autoclave leaching were carried out in stainless steel ball-mills of cylindrical shape under different conditions of temperature, pressure, time and alkali amount and strength. The ball-mills were heated and mechanically rotated in an electric furnace by means of roll mechanism. The effective rotation speed was fixed at 130 rpm in all tests. The charge of steel balls of different diameters was equivalent to 45% of the total mill volume. Monazite was charged in ball-mill without preliminary grinding. It is found that high rate of monazite leaching by ball-milling leaching method is achieved at lower temperature, shorter time and lower expense of alkali than in autoclaves. The results obtained show that complete recovery of thorium and lanthanides from monazite (99.8%) by simultaneous ball milling and alkaline leaching is attained at 140°C within 2 h. It is concluded that processing of monazite by its simultaneous ball-milling and leaching is mechanically activated and accelerated as a result of grinding action of steel balls that caused the continuous removal of the hydroxide product from reacting particle surfaces. This leads to the exposing of fresh and activated monazite particles surfaces to alkali leach solution and consequently the acceleration of the reaction of monazite processing.

Jan 1, 2006

By K. L. Money, R. R. Bleakney, R. H. Hanewald

The processing of EAF baghouse dusts, rolling mill scales, and belt grinding swarfs from the specialty steel industry will be reviewed. In addition, the INMETCO process has been modified so as to recover nickel, chromium and iron from many other waste materials such as pickling solutions, filter cakes, spent nickel and chromium plating baths, super alloy wastes, and nickel-cadmium batteries. INMETCO is the only North American company presently capable of recycling nickel-cadmium batteries by high temperature metals recovery.

Jan 1, 2000

By Mariane Costalonga de Aguiar, Carlos Mauricio Fontes Vieira, Sergio Neves Monteiro

"This work evaluates the effect of incorporation of an ornamental rock waste into an industrial clayey body used for roofing tiles fabrication. Formulations with 0, 10, 20 and 30 wt.% of waste were prepared by replacing the sand in the industrial clayey body. The plasticity of the formulations was determined by the Atterberg limits. Specimens were fabricated by 18 MPa press-molding and then fired from 850, 950 and 1050°C. The specimens were tested to determine the water absorption, linear shrinkage and three points bending flexural strength. The results indicated that the waste improves the extrusion performance of the clayey body by decreasing its plasticity. The use of the waste was beneficial to the water absorption and mechanical strength of the fired clayey ceramic at 1050°C.IntroductionOrnamental rock is a natural resource available in the municipal area of Santo Antonio de Padua and located 150 km from the city of Campos dos Goytacazes, northe of state of Rio de Janeiro, Brazil. Intense industrial activity related to ornamental stones, especially gneisses, is traditionally occurring in the region. After mining, the flagstone is submitted to sawing to obtain blocks and then, after a manual operation, the final products are small flagstones [1,2]. During the sawing operation, a sludge composed of water and fine particles of rock is generated. A monthly production of 1000 tons of ornamental rock waste is estimated to be produced at Santo Antonio de Padua. The final disposal of this waste has brought serious environmental problems. Since most industries do not have an adequate sludge treatment, the waste is contaminating the soil and underground waters as well as obstructing rivers and lakes.Ceramic bodies industrially fabricated in the municipal area of Campos dos Goytacazes, 280 km from the city of Rio de Janeiro, are still empirically elaborated using a mixture of local clays. These clays are predominantly kaolinitic mineral, associated with high plasticity. Due to the excessive plasticity of the ceramic bodies, it is common to have dimensional defects in the final products after the drying and firing processes. Moreover, the kaolinitic structure and the presence of aluminum hydroxide confer a refractory behavior to the local clays. This impairs sintering during the firing operation. In the case of clay ceramics for civil construction, this results in greater porosity associated with elevated values of water absorption [3,4]. To avoid this problem, it is necessary to reformulate the ceramic body composition. The addition of both non-plastic materials to reduce plasticity and fluxes to condition the refractoriness is a possible alternative."

Jan 1, 2011

By Raj Mutharasan

The phenomena of gas-molten metal reactions for the production of metal matrix composites consist typically of a combination of one or more gas transport steps and a liquid gas reaction step. Reaction products include such strength enhancers, grain refiners, or high thermal conductivity phases as TiC, AIN, SIC, Si3N4, TiN in aluminum alloys. Nitrides, carbides and oxides can be produced at various volume fractions and in fairly fine sizes (500 am to 5 um) in laboratory melts by Reactive Gas Injection method (RGI). Gas injection methodology to produce the reinforcements is attractive because it can potentially be scaled to production scales in excess of 10,000 kg/h. For continuous production, the reactant molten metal can be continuously fed into the .crucible where the reactive gas is injected. The molten metal phase reactant may also be involved in a controlling transport step, depending on its concentration and viscosity. It is well known that the reaction product reinforcement size and shape of these phases have significant impact on the physical, mechanical and thermal properties. The current state of knowledge is unable to predict the kinetics and growth of solid reaction products obtained. The primary goal is to develop a fundamental framework for the understanding and prediction of the particle size in such reaction systems. In addition, the role of gas transport, liquid hydrodynamics and decomposition are important issues. A reaction-transport model is being developed using a reaction, transport, and thermodynamic framework, both at macro and at atomistic level to assess gas - liquid interactions.

Jan 1, 1996

By Yanhui Liu, Xuewei Lv, Pingsheng Lai, Chenguang Bai

The purpose of this paper is to study the effect of slag basicity on the Si content in stainless steel master alloys prepared by smelting reduction of Fe-Ni-Cr sinters. Theoretical analysis focusing on the gas, slag and alloy phases of the smelting reduction process at 1600°C was carried out by thermodynamic calculation software----FactSage, showing that the increase of CaO within the slag can result in the decrease of Si within the master alloy. Experiments were also carried out in vacuum melting furnace at 1600°C , and chemical analysis method was used to detect Si content in the alloys. When the MgO content is 9.00%, the experimental results were consistent with the calculated values. However, when the MgO content rises up to 14%, the content of Si in the alloy reaches the maximum when SiO2 equals to 22.81%.

Jan 1, 2016

By John A. Herbst

Plantwide control of mineral processing operations has long been sought for its potential benefits. These benefits include minute-to-minute optimization, reacting to disturbances in ore characteristics and equipment status as they happen and the coordination of all unit operations in pursuit of the highest performance level. However several difficult challenges have kept us from fully realizing those benefits. One of these challenges has been to provide fairly complete quantitative descriptions of Unit operations to account for critical interactions within and 'between unit operations. In some cases we understand the physics and chemistry very well and can incorporate that 'knowledge into phenomenological models. In other cases our knowledge is incomplete, so we must rely on other forms of knowledge such as fuzzy logic or neural nets. Another challenge to be met has been to simultaneously compute a large number of manipulated variables. In the past this challenge was met by optimizing only unit-by-unit, rather than on a global basis to significantly reduce the number of variables. In this paper, a procedure that globally optimizes one or two important variables is outlined. This procedure comes much closer to true plantwide optimizing control while remaining computationally feasible. Finally, another major challenge is to choose a meaningful global objective that can be calculated With the models and can be effectively optimized. Financial goals seems to be the objectives of choice. This paper discusses recent progress In overcoming the challenges and illustrates a promising approach which is being pursued at :Mexicana de Cobre's 'La Caridad copper ore concentrator. At M de C, advanced ,control strategies have been 'installed one at a time in the crushing, grinding and flotation sections. During this period, the throughput of La Caridad, Mexico's largest copper concentrator, 'increased from 76;000 tpd to 90,000 tpd. Plantwide integration is expected' to gain an additional 3% improvement in profitability.

Jan 1, 1996

By Jong-Ren Tarng, Gin-Hwa Chen, Wen-ku Chang, Ke-Ming Lin, Yuan-Haun Lee

"The majority of early studies used X-ray diffraction, but this requires a model to interpret the diffraction processes. A turbostratic model has been applied by Warren, Franklin and Bacon to a wide range of materials including both soft and hard carbons. Maire and Mering applied the same methods to the interpretation of the (001) lines of a series of graphitic carbons. In our case, graphitic carbons undergone high temperature and high pressure graphitization processes have been evaluated by the same methods. It were found that most technological XRD data were obtained by a Rietveld method with the least-squares refinements could be in the simplest way since the full correction technique is very laborious. The behavior of carbon materials as it proceeds through the graphitization process is characterized by changes in the measured interlayer spacings (d) a~ a function of temperature. A series of graphitic carbons including the transformation of diamond to graphite through the process under high temperature and high pressure have been evaluated. A simple calibration equation has been established. IntroductionRecently, in battery industry, carbon materials are used as cathode in lithium ion batteries. However, graphitization of those carbon materials is concerned as if lithium ion intercalated into those carbon cathode. Both high-graphitization and low-graphitization carbon materials are suitable for this kind of application.As for graphitization, the starling materials from which carbons may be prepared vary extensively from pure chemical compounds, to mixtures containing II wide range of molecular weights, such as pitches. So its graphitizing, perhaps the most notable feature of the process, is the very wide range of temperature over which the perfection increase, unlike the more common transformations of solid state materials which occur in a narrow temperature range. The variables involved in the conversion of the initial hydrocarbon to a carbon residue, which may vary widely in final perfection, are time, temperature, stress and impurity content"

Jan 1, 1996

By William Petrul

Image analysis studies were performed on mill products from laboratory flotation tests of the Zn-Pb ore from the Faro deposit in Yukon, Canada, to determine mineral liberations at specific grinds and to predict recoveries at optimum flotation conditions. The minimum and optimum grinds for liberating sphalerite and galena were predicted from size analysis data for the minerals in large ore pieces, and determined by image analysis studies of the mill products. The determined optimum grinds are about 2 Tyler mesh sizes larger than predicted because sane of the fine grained sphalerite and galena occurs in interstices between coarser grained pyrite and is liberated when the pyrite grains are broken apart. Materials balance calculations were performed on the analyzed values for the liberated and unliberated sphalerite and galenaa to determine their distributions in the mill products. The laboratory flotation tests recovered 74% of the sphalerite and 83% of the galena in Zn and Pb concentrates respectively. The mineral evaluation study indicates that the optimum recovery for sphalerite and galena are 85 and 83% respectively. The company is currently recovering 80% 'of the sphalerite and 82% of the galena.

Jan 1, 1989

By T. Ueno

Naoshima Smelter & Refinery of Mitsubishi Materials Crop. commissioned a new Mitsubishi continuous copper smelter in May 1991. Process offgas volume of the conventional reverberatory furnace line, one of the previous smelters having been shut down, was very large and thus two acid plants had been operated. It was expected that the offgas volume would be reduced at the new smelter to about a half of the sum of those from previous two 1 smelters and the sulfur dioxide strength would be increased. So various alternatives were studied to minimize the operation cost. And it was decided to utilize both of the plants with minor modifications by diluting the gas either with air or with dilute gases. The acid plants now receive offgases from the new copper smelter, a sintering machine of a lead smelter and a decomposer of waste acid. The paper discusses plant design, operation, improvements and modifications realized in relation with the retrofitting of the copper smelter.

Jan 1, 1992

By Susanne Pignolet-Brandom

Reflected light microscopy, and scanning electron microscope energy dispersive spectroscopic analysis and backscatter electron images were used to determine if a "slick dross" with undesirable handling properties has an assemblage of phases distinct from normal dross. This study has found that in the normal dross the most abundant lead phases are lead sulfide and lead metal and the most common copper phases are copper-iron sulfide and copper sulfide. In the slick dross, the most abundant copper phase is copper-lead sulfide and the most common lead phases are copper-lead sulfide and lead sulfide. The resulting mineralogical information has provided additional insight into the causes of the handling problem and the reaction mechanism for the formation of normal and slick dross

Jan 1, 1988

By M. Opler

Presently, only a few large copper refineries are able to produce Grade A cathodes from copper scrap. Today's technology needs large plants for smelting, converting or refining the main impurities and casting the anodes for electrolytic refining. A new ECUPREX® PROCESS, by-passes all pyrometallurgical operations and produces directly copper cathodes starting from copper scrap with high lead and tin contamination. Copper scrap from chopped cables, copper cements and electronic scrap are suitable feed for ECUPREX® PROCESS. This process uses a non-conventional electrolyte and produces a surprisingly high quality, smooth cathode assaying only few ppms of total metallic impurities. Bench-scale work followed by a successful mini-pilot plant run, has led to the construction of an operating pilot plant equipped with a 1,000 Ampere cell. The results of the operations of this pilot plant are presented and described in this paper.

Jan 1, 1995

By John A. Herbst, William T. Pate

"Plantwide control of mineral processing operations has long been sought for its potential benefits. These benefits include minute-to-minute optimization, reacting to disturbances in ore characteristics and equipment status as they happen, and the coordination of all unit operations in pursuit of the highest performance level. However, several difficult challenges have kept us from fully realizing those benefits. One of these challenges has been to provide fairly complete quantitative descriptions of unit operations to account for critical interactions within and between unit operations. In some cases we understand the physics and chemistry very well and can incorporate that knowledge into phenomenological models. In other cases our knowledge is incomplete, so we must rely on other forms of knowledge such as fuzzy logic or neural nets. Another challenge to be met has been to simultaneously compute a large number of manipulated variables. In the past this challenge was met by optimizing only unit-by-unit, rather than on a global basis to significaritly reduce the number of variables. In this paper, a procedure that globally optimizes one or two important variables is outlined. This procedure comes much closer to true plantwide optimizing control while remaining computationally feasible. Finally, another major challenge is to choose a meaningful global objective that can be calculated with the models and can be effectively optimized. Financial goals seems to be the objectives of choice.This paper discusses recent progress in overcoming the challenges and illustrates a promising approach which is being pursued at Mexicana de Cobre's La Caridad copper ore concentrator. At M de C, advanced control strategies have been installed one at a time in the crushing, grinding and flotation sections. During this period, the throughput of La Caridad, Mexico's largest copper concentrator, increased from 76,000 tpd to 90,000 tpd. Plantwide integration is expected to gain an additional 3% improvement in profitability."

Jan 1, 1996

By Pekka Hanniala

The Outokumpu Flash Smelting process today is the most feasible method for copper matte smelting. The economic feasibility of the process has always been one of the main decision making criteria in smelter projects. Thus, today about 50 % of the world primary copper production utilizes Outokumpu Flash Smelting Technology. However, in the future, environmental criteria will have stronger and stronger impact on decision making. Flash Smelting technology offers the best pollution control features of any process. today. It is foreseen that, in the near future, the global trend will be that all the smelters must decrease their emissions at an accelerating rate, compelling the smelters to make increasingly larger investments on environmental protection. In most of smelters ?today, Peirce-Smith converting and transfer of the molten material in ladles are the number one pollution source. The key today for copper converting and minimizing emissions is the Kennecott-Outokumpu Flash Converting process, which has proven to be the most effective converting method in terms of pollution control and, production efficiency including capital and operational costs. Outokumpu Flash Smelting technology is applicable also for small to medium scale smelters but the most interesting area is the upper capacity limit for smelting in one line, which has not yet been reached. We predict that by the year 2000 to 2005, there will be at least one smelter which produces 500,000 tonnes of Cu per year based on one Flash Smelting and Flash. Converting unit. The current state-of-the-art of the Outokumpu Flash Smelting - Flash Converting process is presented in this paper as well as some new options for copper production to be utilized in the near future but which are available already today.

Jan 1, 1998

By J. B. W. Bailey

The Noranda Horne smelter in Quebec, Canada has change considerably during the last two decades to accommodate varying custom concentrate receipts, closure of the Horne mine, better working conditions, environmental programmes, new technology and increased energy and labour costs. This paper highlights the reasons for changing the smelter from two calcine charged and one wet charge reverberatory furnaces fired by coal to a smelter using. tonnage oxygen oil, natural gas and coal in a single wet charged reverberatory furnace and a Noranda Process continuous Reactor. The current operation 1 described, including three major topics; the use of oxygen/fuel burners on the charge banks of the reverberatory furnace which has increase the smelting rate from 680 to 1100 tonnes of concentrate per day; the oxygen enrichment of the Noranda Process converting air to achieve smelting rates of over 1800 tonnes of concentrate per day; the converting of the mixture of 73 percent copper matte produced from the Noranda Process and the 33 percent copper matte produced from the reverberatory furnace.

Jan 1, 1983

By Carlos Maurício Fontes Vieira, Sergio Neves Monteiro, Diogo Neves Henriques

"This work evaluates the effect of incorporation of an ornamental rock waste into an industrial clayey body used for roofing tiles fabrication. Formulations with 0, 10, 20 and 30 wt.% of waste were prepared by replacing the sand in the industrial clayey body. The plasticity of the formulations was determined by the Atterberg limits. Specimens were fabricated by 18 MPa press-molding and then fired from 850 to 1100oC. The specimens were tested to determine the water absorption, linear shrinkage and three points bending flexural strength. The results indicated that the waste improves the extrusion performance of the clayey body by decreasing its plasticity. The use of the waste was beneficial to the water absorption and mechanical strength of the fired clayey ceramic at temperatures above 1000 ° C.IntroductionOrnamental rock is a natural resource available in the municipal area of Santo Antônio de Pádua and located 150 km from the city of Campos dos Goytacazes, northe of state of Rio de Janeiro, Brazil. Intense industrial activity related to ornamental stones, especially gneisses, is traditionally occurring in the region. After mining, the flagstone is submitted to sawing to obtain blocks and then, after a manual operation, the final products are small flagstones [1,2]. During the sawing operation, a sludge composed of water and fine particles of rock is generated. A monthly production of 1000 tons of ornamental rock waste is estimated to be produced at Santo Antônio de Pádua. The final disposal of this waste has brought serious environmental problems. Since most industries do not have an adequate sludge treatment, the waste is contaminating the soil and underground waters as well as obstructing rivers and lakes.Ceramic bodies industrially fabricated in the municipal area of Campos dos Goytacazes, 280 km from the city of Rio de Janeiro, are still empirically elaborated using a mixture of local clays. These clays are predominantly kaolinitic mineral, associated with high plasticity. Due to the excessive plasticity of the ceramic bodies, it is common to have dimensional defects in the final products after the drying and firing processes. Moreover, the kaolinitic structure and the presence of aluminum hydroxide confer a refractory behavior to the local clays. This impairs sintering during the firing operation. In the case of clay ceramics for civil construction, this results in greater porosity associated with elevated values of water absorption and low mechanical strength [3,4]. To avoid these problems, it is necessary to reformulate the ceramic body composition. The addition of both non-plastic materials to reduce plasticity and fluxes to condition the refractoriness is a possible alternative."

Jan 1, 2008

By Qiu Dingfan

The Slurry Electrowinning Process (SEP) is a new hydrometallurgical method and clean technology, Sulfide ores can be treated by the SEP without S02 emission and the sulfur from the sulfides can be recovered in element form which is easy to stockpile and can be transported at low cost. In a special slurry electrowinning cell one can achieve at the same time the leaching of elements from the feed and the electrowinning of metals from the electrolyte, Because the anode reactions are utilized for leaching of some elements the consumption of the energy is decreased, SEP also has the advantage of separation some elements, It is especially suitable for treatment of complex concentrates containing Pb, Cu, Au, Ag and S, which could hardly be accepted by any smelter. In this work, the behavior of different metals in this process has been studied and it was found that the separation of metals in some minerals is possible through the SEP, Beijing General Research Institute of Mining and Metallurgy (BGRIMM) has studied the possibility of the SEP to treat bismuth concentrates containing S, Be and F in laboratory and pilot-test scale as well as in commercial plants, The commercial plant was set up in 1997, It has been in operation since that time, According to the results of laboratory experiments and pilot- plant test, a new plant to treat complex gold minerals was set up in 1998 and is in operation in 1999

Jan 1, 2003