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By C. R. Palmer

The Bureau of Mines investigated the use of ion-exchange technology for the recovery of precious metals from cyanide leach and spent electrolytic solutions. This research included adsorption of gold and silver on both weak-and strong-base anion-exchange resins. The effects of nickel, mercury. and iron on precious metal loading of strong-base resins were also determined. Due to the nonselectlvity of strong-base resins, selective elution also was investigated. Both commercially available and experimental weak-base anion-exchange resins were tested. None of the commercial weak-base resins tested were suitable for a caustic-cyanide system owing to their low recovery of precious metals at pH 10 or above; however, three experimental resins have possible application. Continuous tests conducted with mill cyanide solution in a multicompartmented ion-exchange column using strong-base anion-exchange resins adsorbed nearly 100 pct of the precious metals as well as the iron and nickel. During the elution of this loaded resin the iron was first removed with NaCI plus NaOH; then nickel with dilute H2S04 or HCl; finally gold and silver with thiourea in dilute HCl.

Jan 1, 1988

By Christian Ludwig, Virginie Silberstein, Rizlan Bernier-Latmani, Simona Regenspurg

"Residues from waste incineration (bottom ashes) form large amounts of heavy metal-rich waste. Theoretically, heating and the addition of chloride to the ashes could remove these metals by formation of volatile metal chlorides. The remaining heavy metal-poor ashes could be used, for example, as cement additives. In the proposed process of our study we used bypass dust from the cement industry as chloride additives to the bottom ashes. We aim to determine experimentally the optimal conditions to remove heavy metals from ashes and to simulate this process by thermo- chemical modeling. In our experiment we investigate heavy metal flows by heating of differently composed mixtures of bottoms ash and bypass dust in dependence of different furnace temperatures (500-1200 °C). Furthermore, we investigate the reactivity (leaching characteristic) of the resulting product in order to predict if secondary residues can be landfilled in agreement to Swiss regulations for inert materials.IntroductionThe incineration of garbage is generally considered as the most environmentally friendly method for the reduction of municipal solid waste. This is because, compared to traditional storage of waste on landfills, incineration produces less greenhouse gases and destroys toxic organic compounds. The released exothermic energy can be recuperated and the residues from the combustion chamber (bottom ash) are strongly reduced in volume. However, they still form about 600 kt of waste per year in Switzerland, which needs to be landfilled. However, these residues could be potentially used as construction materials after mechanically recovering ferrous and non-ferrous metals. However, the resulting ashes (discharged dry or wet) still contain increased amount of heavy metals (exceeding state regulation) requiring them to be finally deposed on a hazardous waste site. A thermal treatment of these ashes could enable both, to separate and recuperate the remaining heavy metals and an inorganic heavy-metal poor material. The evaporation of metals depends on temperature and can be lowered by addition of chlorides, which would lower the boiling point of most metals by formation of metal chlorides (table 1). 745"

Jan 1, 2008

By Christian Ludwig, Virginie Silberstein, Rizlan Bernier-Latmani, Simona Regenspurg

"Residues from waste incineration (bottom ashes) form large amounts of heavy metal-rich waste. Theoretically, heating and the addition of chloride to the ashes could remove these metals by formation of volatile metal chlorides. The remaining heavy metal-poor ashes could be used, for example, as cement additives. In the proposed process of our study we used bypass dust from the cement industry as chloride additives to the bottom ashes. We aim to determine experimentally the optimal conditions to remove heavy metals from ashes and to simulate this process by thermo- chemical modeling. In our experiment we investigate heavy metal flows by heating of differently composed mixtures of bottoms ash and bypass dust in dependence of different furnace temperatures (500-1200 °C). Furthermore, we investigate the reactivity (leaching characteristic) of the resulting product in order to predict if secondary residues can be landfilled in agreement to Swiss regulations for inert materials.IntroductionThe incineration of garbage is generally considered as the most environmentally friendly method for the reduction of municipal solid waste. This is because, compared to traditional storage of waste on landfills, incineration produces less greenhouse gases and destroys toxic organic compounds. The released exothermic energy can be recuperated and the residues from the combustion chamber (bottom ash) are strongly reduced in volume. However, they still form about 600 kt of waste per year in Switzerland, which needs to be landfilled. However, these residues could be potentially used as construction materials after mechanically recovering ferrous and non-ferrous metals. However, the resulting ashes (discharged dry or wet) still contain increased amount of heavy metals (exceeding state regulation) requiring them to be finally deposed on a hazardous waste site. A thermal treatment of these ashes could enable both, to separate and recuperate the remaining heavy metals and an inorganic heavy-metal poor material. The evaporation of metals depends on temperature and can be lowered by addition of chlorides, which would lower the boiling point of most metals by formation of metal chlorides (table 1)."

Jan 1, 2008

By Hong Peng, James Vaughan

Thermal activation of bauxite has been proposed to enable bauxite dissolution at a reduced digestion temperature and also to reduce the organic content in the liquor. Research has been carried out on phase transformation of its main hydroxide components (gibbsite, boehmite and kaolinite) during calcination. However, there is limited information available on phase bauxite phase transformation during thermal activation. In this study, two bauxite ore samples were heated from 25 to 700 °C at a rate of 50 °C/min while monitoring the phase transformation using Rigaku in situ XRD. Different phase transformation pathways for gibbsite in the bauxite compared with pure gibbsite was observed. Boehmite and kaolinite in bauxite behaved similarly to their pure phases. The temperature of phase transformation depends to some extent on the bauxite sample. Samples were also characterised by scanning electron microscopy (SEM) to reveal changes in the microstructure.

Mar 1, 2018

By D. C. Azubike

Wolframite (FeWO4) usually having cassiterite (SnO2) as a major impurity is a primary source of tungsten. Its direct reduction/carburisation with carbon in the temperature range 1000-1400°C, and with hydrogen at 600-900°C followed by carburisation with CO at 900°C are described. Depending on the conditions and reactants employed, Fe, Fe2W, B-Sn,WC, W2C, Fe3W3C and Fe6W6C are the products. Tin was found to inhibit the overall reduction and carburisation reactions significantly. The potential for either efficient separation of iron and tungsten or a one-stage production of an iron-based metal carbide composite is discussed.

Jan 1, 1992

By Peter Willbrandt

The flash smelter at NA was commissioned in March 1972 with an initial throughput of 50 tons of dry copper concentrate per hour. As a result of various measures, for example, oxygen enriched process wind, extension of the radiation part of the waste heat boiler, etc., the throughput could be increased to the present 70 tons per hour of dry concentrate. NA's plant is located on the outskirts of the city of Hamburg. The flash smelter's location and the growing awareness of the German population as regards environmental issues necessitate again and again considerable capital expenditure being spent on environmental protection. Thanks to the numerous small and large measures taken to protect the environment the emissions of dust, heavy metals such as arsenic, copper, lead, etc., and as well SO, could be drastically reduced. This paper will be giving an overview on the present state of the flash smelting process and the impact of the increasing environmental awareness at NA.

Jan 1, 1993

By Jan Vrestal, Josef Tomiska, Pavel Broz

"Thermodynamic investigations on fcc solid ternary Fe-Ni-Cr alloys have been performed by means of the computer-aided Knudsen cell mass spectrometry. Ternary T.AP.-series (Thermodynamically adapted power series) are used for the algebraic representation of the thermodynamic excess properties. At 1650 K the molar excess Gibbs energy GE is negative over the whole field of stable fcc phase. The molar heat of mixing HE is exothermic in the predominant part of the fcc phase field. Only between the section with a constant ratio of mole fraction Xcr/XNi = 0.64 and the fcc phase field boundary the HE values are slightly endothermic. The results of this work can be used successfully for phase diagram calculations.IntroductionThermodynamic investigations on multicomponent alloy systems such as the Fe-Ni-Cr ternary system including the three binary boundary systems are very time-wasting and usually beset with considerable experimental difficulties. Additionally, the required experimental equipment is very expansive and the obtained results are not always satistying. Therefore it is understandable that many phase diagram calculations are based only on few experimental values of the molar excess free Gibbs energy GE. Consequently, Kundrat and Elliott [1] as well as Hillert and Qiu [2] used in their reassessments of the phase diagram of the Fe-Ni-Cr system thermodynamic data mainly assumed and/or optimized by means of various reasoning.Lee [3] reported recently, a revision of the used thermodynamic description of the Fe-Ni liquid phase is necessary to obtain a better agreement with the experimental data on the bcc/liquid or fcc/liquid tie lines and liquidus temperatures in the Fe-rich region of the Fe-Ni-Cr ternary system than in the previous assessments. This is 'in full agreement with mass spectrometric investigations of Fe-Ni alloys in the liquid and in the fcc solid phase, published earlier [4,5]. Indeed, phase diagram calculations based upon the molar excess free Gibbs energies GE obtained in these studies yield liquidus and solidus lines in excellent agreement with experimental phase diagram data [5]. Nevertheless, these experimental data have not been considered later on any more, not even in the revision by Lee [3]."

Jan 1, 1996

By M. Cassir

"The unique properties of molten carbonates offer a large scope of applications in the field of energy. In effect, these molten salts are in the center of chemical and electrochemical reactions involving carbon and carbonaceous species, carbon dioxide and carbon monoxide, significant for energy generation or even for the production of fuels. Moreover, such media have also an oxidative character; they dissolve molecular oxygen and oxygen reduced species, O 2-, O22- and hypothetically o-, which may have an important role in waste treatments, homogeneous catalysis and synthesis of oxides. In this presentation, an overview will be given on the principal physicochemical properties of molten carbonates, before focusing on their main known application, the molten carbonate fuel cell (MCFC). Progress in other new fuel cells applications will also be analyzed, such as direct carbon fuel cell (DCFC), hybrid carbon fuel cell (HDCFC) and composite high-temperature fuel cells combining the features of MCFC and solid oxide fuel cell (SOFC). Afterwards, membranes for the separation and capture of C02 will be reviewed. Finally, other topics, as the oxidative coupling of methane in molten carbonates, will be briefly mentioned.IntroductionIn the thirty past years, the molten carbonate science and advances have been mainly dedicated to the understanding and optimization of the molten carbonate fuel cell (MCFC), which is still a major issue in the heart of a new vision of energy development. More recently, new topics related to other kinds of fuel cells (DCFC, composite SOFC/MCFC systems) and C02 capture have emerged and are concentrating important research and technological efforts. Moreover, new fields of implementation, related to molten carbonates, are also present: geology, glasses, production of nanocarbon particles etc. Considering other areas where this molten phase plays a major role, such as catalysis, waste destruction, surface treatment, it can be confirmed that the field of molten carbonates is very rich and offers many opportunities for fundamental science and competitive applications. Whatever their specific application, molten carbonates activity is associated to more efficient energy systems with low production of C02 and, in a prospective sense, to non-polluting energy using the value of C02. A recent event, the International Workshop on Molten Carbonates & Related Topics, IWMC201 I, held in Paris in 2011 , have put in evidence the importance to improve and exploit this investigation and technological domain."

Jan 1, 2012

By M. Neises, M. Roeb, C. Sattler, S. Stenger

"A two-step thermo-chemical cycle process has been developed and investigated. It is based on metal oxide redox pair systems, which can split carbon dioxide as well as water molecules by extracting oxygen atoms and reversibly incorporating them into their lattice. If concentrated solar radiation is used as the heat source, a promising method exists to produce synthesis gas from water and CO2. An easy way of operation is gained by the combination of a ceramic substrate as the absorber structure, which can be heated to high temperatures with concentrated solar radiation, and of a metal oxide coating which is capable to carry out the redox reactions. The performance and kinetics of a ferrite based redox material coated on ceramic substrates were investigated in a laboratory set-up. CO2 could be reduced with significant conversions. In addition, several side reactions were observed like the formation of carbon and like the Boudouard reaction.IntroductionThe search for alternative energy carriers and for processes able to reuse carbon dioxide stimulates the research for sustainable routes of alternative fuel production. In the scope of this search thermo-chemical processes combined with sources of concentrated solar energy have become more and more attractive. Ideally, the only raw materials for such processes are water (H2O) and carbon dioxide (CO2) enabling not only a process free of emissions, but also allow to reduce emissions of other processes by reusing CO2 to provide synthesis gas, which itself can be applied to produce chemical commodities or even better synthetic fuels like methanol or petrol.In contrast to the direct splitting of those raw materials, thermochemical cycles split water and CO2 in several steps and enable hydrogen (H2) and carbon monoxide (CO) generation at temperatures controllable by today’s technical equipment. One of the most interesting thermochemical cycles is a two-step process using metal oxide based redox systems. During the first step of this cycle (the regeneration step) the metal oxide is reduced setting some of its lattice oxygen free according to reaction (1). In the next step (the splitting) the reduced and activated material is oxidised by withdrawing oxygen from water and CO2 and at the same time hydrogen and CO is set free according to reactions (2a) and (2b) respectively."

Jan 1, 2011

By C. P. Broadbent

Due to growing .public awareness of environmental issues and greater sensitivity towards waste management, many countries around the world are implementing more stringent legislation governing the storage and disposal of hazardous wastes containing heavy metals such as As, Sb, Pb, Cd or Hg. These wastes can no longer be dumped without providing clear guarantees that the material concerned is environmentally safe and will not leach toxic elements to the surroundings. In the Netherlands the current dumping charge for chemical waste (i.e. worst category) is $280/t, and for industrial waste this cost reduces to $75/t. If the material can be reused there may be a small positive credit for selling it, for example discard slag as an aggregate to the construction industry. A number of (pyre)-metallurgical operations, mostly associated with the extraction of metals from sulphidic ores, produce arsenic residues in the form of As2O3 containing flue dusts and speises. If the flue dust is of high purity it can be sold, though many traditional uses are being substituted by other materials. In many cases upgrading the quality of the arsenical dusts is not possible for either technical or economic reasons. Traditional practice is to dissolve these dusts in acid prior to precipitation as ferric arsenate, which is at present classified by many countries as industrial waste and can be dumped. Recent work, however, has cast doubt on the stability of arsenates for disposal and alternative disposal routes have been investigated. Tests have shown that up to 10% (dm) As can be incorporated into "glassy" silicate slags with very low levels of arsenic leaching in the cooled product. Calcium arsenate was added to a range of synthetic and industrial slags from the system SiO2-FexOy-CaO-A12O3-AsmOn, under mildly oxidising conditions and quenched subsequently in water. It would appear that this represents an environmentally acceptable method for the disposal of many arsenical residues and there is some optimism that this method will be equally applicable to the disposal of other toxic metal residues.

Jan 1, 1994

By R. C. Chaturvedi, S. B. Padwal

"Padwal and Chaturvedi have developed the model based on M-K theory, considering Hosford's yield criterion and critical thickness strain criterion"" to predict the sheet metal forming limits under simple (constant) strain ratio paths. This analysis has been extended in this paper to predict the sheet metal forming limits under complex strain paths. The effects of exponent ""a"" in Hosford's yield criterion and strain paths on the forming limits under complex strain paths are studied using this analysis. The predictions of the present analysis are compared, both for simple and complex strain paths, with experimental results of Ishigaki for A.K. steel and also with the predictions of Rao and Chaturvedi's model. The quantitative analysis of the error in predicting the forming limits has also been carried out using a method suggested by the authors earlier.1. INTRODUCTIONThe constant strain ratio condition has been assumed in the theories developed for prediction of forming limit diagrams (FLO). In actual forming operation, this condition is seldom satisfied. Even in the case of simple single stage press formed components, the strain path becomes curved and non-linear. In the case of pressings with complex shapes, or multiple stages of forming, the changes in strain path are more pronounced and even abrupt.Experimental study of the forming limits, under two stage strain paths, by Ishigaki [1], has shown that the forming limits are path dependent. It has been observed that the forming limits lower than that under simple strain paths, may be obtained under certain strain paths (when the first stage strain path is either equibiaxial tension or uniaxial tension, followed by the second stage strain path as plane strain). Rasmussen's work [2J, on the theoretical study of forming limits under curvilinear strains paths, has shown that a large drop in formability can result from very small changes in strain path. Thus if a deformation process gives rise to failures due to plastic instability, the failure is not necessarily due to insufficient formability of the material. In such cases, FLOs based on constant strain ratio path should not be used directly in predicting the success or failure of the forming operation. Thus the knowledge of forming limits under complex strain paths is of great importance to the interpretation of press-shop problems."

Jan 1, 1994

By Corby G. Anderson

Today, with a stringent economic and environmental climate prevailing in the copper business, there is increased interest in evaluating new processing alternatives for production. Hydrometallurgical pressure oxidation of copper concentrates is one of the more viable approaches and several technological candidates have emerged. Of these, an overlooked but industrially proven methodology utilizing nitrogen species catalyzation in the oxidizing pressure leach system may prove to be a feasible process alternative for the future. In this paper, the history of the system and its application to chalcopyrite concentrates will be outlined. In particular, a methodology for effective treatment of precious metals bearing chalcopyrite concentrates via partial oxidation at low temperatures and pressures will be discussed. Finally, the perceived economics of this unique industrially proven process will be delineated.

Jan 1, 1999

By William Petruk

Many gold operations lose gold during processing because some ore characteristics which affect recoveries have not been determined, and consequently the plant could not be designed to account for them. The ore characteristics can be determined with mineralogical techniques by analyzing the plant feed, final tailings and mill products. The plant feed and/or final tailings are commonly analyzed first as a separate project. Mill products are analyzed only if the process employs a minerals separation circuit to produce a concentrate (e.g. secondary flotation circuit to concentrate gold-bearing arsenopyrite), and if assays and materials balances indicate a recovery problem in the minerals separation circuit. Many ores have been evaluated at CANMET on a confidential cost-recovery basis by custom-designing a work plan which was dependent upon the problem and on the characteristics of the ore. The reasons for gold losses have been identified in most cases, and suggestions for modifying flowsheets have been proposed. The methods used in performing the analyses are described in this paper, and non-confidential results from in-house projects are provided as examples of the benefits of such analyses. The analytical methodology involves a combination of the following procedures: -producing heavy mineral concentrates and identifying the gold minerals in the concentrates; -determining quantities of invisible gold in gold-bearing sulphides, sulpharsenides, etc. by SIMS; -determining quantities and liberation characteristics of all gold minerals and gold-bearing minerals in the sample; -finding and identifying gold minerals in silicates; -extensive grinding and cyanidation to determine the ultimate amount of cyanidable gold; -determining impact of clay minerals and graphite; -performing a mineral balance for the gold in each sample; -performing a materials balance to determine the distribution of the gold minerals, gold-bearing minerals, and other minerals throughout the flowsheet, and; -interpreting the results.

Jan 1, 1995

By Seung-Chul Lee

Transparent conducting tin(1V) oxide thin films have been studies and developed for the electrode materials of solar cell substrate. Fabrication of tin oxide thin films by sol-gel method is process development of lower cost photovoltaic solar cell system. The research is focused on the establishment of process condition and development of precursor. The precursor solution was made of tin isopropoxide dissolved in isopropyl alcohol. The hydrolysis rate was controlled by addition of triethanolamine. Dip and spin coating technique were applied to coat tin oxide on borosilicate glass. The resistivity of the thin film was lower than 0.18-cm and the transmittance is higher than 90% in a visible range.

Jan 1, 1999

By Yasumasa Hattori

Fluid flow in a flash furnace concentrate burner was investigated quantitatively in order to improve burner performance. Computational fluid dynamics was utilized for researching fluid flow in a burner port mathematically then its results were reviewed in the commercial flash furnace burner and its calculation results were found to be in good agreement with the actual measurement results. Based on those results, a mathematical fluid flow model for the Sumitomo flash furnace concentrate burner has been developed so as, to improve premixing and combustion efficiency of concentrate in the reaction shaft.

Jan 1, 2002

By Viktor. P. Popov, Oleksandr. V. Derev'yanko, Oleksandr. I. Raychenko

"This paper is devoted to scrutiny problem of obtaining electro-contacts by electro-discharge sintering technology. A new unconventional method of electro contacts production (on Aggraphite base) can yield essential optimization resource.Review of three electro-technological methods of processing contacts materials is presented:- using graphite powder cladded by Ag;- mixture of graphite powder(which is a non-cladded powder) with Ag powder and addition of Fe powder particles;- method of infiltration of melted Ag into graphite piece without deformation and rupture of object.This technological approach can give the possibility to increase of compression strength of electro-contacts materials up to 340 MPa and more under conditions of additional reinforcing components (for example, by Fe).IntroductionThe electric current can be an active ""participator"" of the powder metallurgy technology [l]. At the passage of electric current through powders or some powder mixtures the phenomena including phase transformations arise. Here such effects, which are observed in the Ag-graphite and Ag-Fe-graphite powder mixtures and in the pair Ag-porous graphite, are described.The Ag-graphite composition materials (CM) are used, for example, as electric contacts [2, 3]. Since a material being produced is destined for the contacts it is necessary to take into account the following aspects: commutating current, its character and voltage, active or reactive character of working load, geometrical dimensions of contacts, quantity and frequency of switching on and switching off, pressure on contacts, distance between contacts, method of arc control, surrounding medium, its content, pressure and temperature. Thus, these and, maybe, choice of some other circumstances influence design, materials and production technology of contacts. The range of problems concerned dictates such steps as alloying of contact materials, optimization of structure, selection of kind of graphite, its connection with metal [4-10]. It is expedient to recall the main procedures of the first stage of the conventional technology: dosage of the initial graphite powder and binder-phenolic resin plastic varnish (for example, Bakelite), mixing, densification, thermal treatment, crushing, grinding, sieving, drying, dosage of grained graphite, dosage of the initial silver powder, obtaining of the silver salt solution, settling of salt, filtration, washing, drying of the cladded graphite powder, thermal treatment, obtaining of the graphite powder of particles cladded by silver. The second stage of the convectional technology starts by obtaining of the cladded graphite powder and finishes by annealing of the pressed blanks (Fig. 1)."

Jan 1, 2004

By Gretel Parker

In situ Raman spectroscopic investigations of copper iron sulfides in leach solutions have been undertaken. Coupling potentiodynamic techniques to Raman spectroscopy produces a powerful tool for studying mineral surface response to changing conditions, while ESEM and high-vacuum techniques provide complementary ex-situ information on surface structure and composition. Oxidative acid leaching of chalcopyrite at ambient temperature yielded a product with S-S bonds that were shifted from those seen with covellite, with little evidence of elemental sulfur formation. Leaching of chalcopyrite led to non-homogeneous product distribution. Raman spectroscopy was able to identify the products formed on the mineral surfacein situ while leaching was occurring. Raman mapping and imaging demonstrated a surface distribution of the products which can be related to composition and structure changes of the mineral surface. The surface formed on chalcopyrite after anodic oxidation at 0.570 V vs. Ag/AgCl in 0.1 mol dm-3 HCl undergoes laser-induced transformation.

Jan 1, 2003

By Larry M. Southwick

Pneumatic converting (Bessemerizing) of iron revolutionized the steel industry. Bessemerizing of copper (conversion of copper sulfide matte to copper metal) was proposed at almost the same time, but it was slow in being accepted. The differences between iron and copper converting were great and technical problems were substantial. It took 25 years for the process to become viable and another 25 years before a truly economical solution was found. A major economical and productivity problem was the short life for converter refractory linings. The first converters had acid (silica) linings, which were quickly consumed since silica was a flux for the process. Converters had to be relined at least once per day, a laboriously expensive manual process with only the most rudimentary mechanical aids available to assist. The industry was revolutionized almost overnight when finally a viable basic (magnesite) lining was developed. This lasted 100's of days versus less than one, leading to converters that were easier to operate and which handled larger charges. This change occurred after W.H. Peirce and E.A.C. Smith, with support from the Guggenheim interests, successfully operated a basic lined converter in a copper refinery in Baltimore. While Peirce and Smith are generally given credit for the development and explosive acceptance of this idea, a Pittsburgh industrialist, Ralph M. Baggaley, working in an independent smelter in Butte, Montana, successfully built and operated a basic lined converter four years before they did. In fact, the early support for Peirce and Smith likely occurred because Guggenheim's staff were encouraged after thoroughly examining Baggaley on his earlier successes. The questions of technology primacy between Baggaley and Peirce/Smith are ironically similar to those between Wm. Kelly and Bessemer in converting iron to steel. This paper will review what Baggaley (and other early researchers) accomplished, examine why he (or they) did not receive credit equal to Peirce and Smith and explore what his (their) place should be in the development of successful basic linings. More suspects than a Victorian Whodunit.

Jan 1, 1999

By D. Quattrini

The aim of the present work is to present the gas chromatography (GC) as an alternative method of analysis in the thermal decomposition of calcium carbonate. Therefore, a furnace/GC on-line system was employed to study the kinetics of the reaction, measuring the CO2 produced in the decomposition. One of the advantages of the GC method is the possibility to perform an in-situ characterization and quantification of the gaseous products to obtain kinetic parameters, besides the method is simple and shows a good reproducibility. The decomposition of calcium carbonate was carried out in isothermal conditions at temperatures from 655 to 715°C with nitrogen as purge gas. Several gas velocities were used to determine the adequate flow that minimizes the effect of external mass diffusion as rate controlling step. It was made a preliminary analysis of the sample size influence on the reaction rate. The activation energy of the reaction was determined by Flynn method. The value obtained was in a good agreement with other authors. On the other hand, gravimetric measurements were employed for compare GC results.

Jan 1, 2006

By Hidekazu Nakagawa

We investigated the anodic dissolution behavior of titanium in TMHA-Tf2N molten salt, which has a wide electrochemical window of about 5 V, in order to develop an electrodeposition method for titanium. By etching a titanium electrode in HF?HNO3?H3PO4 solution, the titanium electrode became electrochemically active, and a redox reaction was observed at around -0.15 V vs. I-/I3- in (TMHA-Tf2N)?HTf2N solution. We identified the redox reaction consists of the reduction of the proton and the oxidation of hydrogen. The diffusion coefficient of the proton in TMHA-Tf2N was calculated to be 6.9 10-8 cm2 s-1 at 50 °C from the cathodic peak current in the cyclic voltammogram. Anodic decomposition of the molten salt was not observed up to 6.0 V vs. I-/I3- on titanium electrode, while it was observed at around 2.0 V vs. I-/I3- on platinum and glassy carbon electrodes. Cathodic decomposition of the molten salt was observed at around -3.0 V on the titanium electrode, as well as on the platinum and glassy carbon electrode.

Jan 1, 2006