923 resultados para metal trace analysis
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"Mémoire Présenté à la Faculté des Études Supérieures en vue de l'obtention du Grade de Maîtrise En Droit Option Recherche"
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Coordination chemistry of schiff bases is of considerable interest due to their various magnetic, catalytic and biological applications. Here it describes the spectral characterization of schiff bases and its Mn (II), Cu (II) and Ni (II) complexes. Then synthesis and spectral characterization of Zn (II), Cd (II) and Co (II) complexes of schiff base derived from 3-Formylsalicilic Acid and 1,3-diaminopropane. Then it discusses the synthesis and spectral studies of Copper (II) complexes of 2-Hydroxyacetophenone N-phenyl semicarbazone. Finally it discusses the synthesis and spectral characterization of Co (III) complexes of salicylaldehyde N-phenyl semicarbazone. The preparation and characterization of Cobalt (III) complexes of salicylaldehyde, N-phenylthiosemicarbazone containing hetrocyclic bases phenalthroline and bipyridine. Thiocyanate, azide and perchlorate ions act as coligands. Elemental analysis suggests +3 state for Cobalt. HNMR, IR and UV-visible spectra characterize the complexes.
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This thesis is a modest attempt in assessing the trace metal levels and their behavior in the aquatic environment of Kuttanad, an aquatic system that is severely affected by man’s intervention on natural processes, by study seriously evaluating the levels of trace metals in dissolved and particulate phases and also in the different chemical fractions of the sediments. Understanding of the distributions, variations and transfer processes of trace metals in different environmental phases in the backwaters of Kuttanad is vital for the assessment of the water pollution problems and study the ecology of the area which contributes 20% of the rice production in the State of Kerala. Kuttand is a low-lying, shallow bay formed as a result of geological uplift. The major economic activity is agriculture involving 40% of the population. About 1.5% of the people are engaged in aquaculture. The trace metal distribution in the Kuttand backwaters is considerably influenced by the tropical features of the location and by human activities including agricultural activities and construction of salinity barrier. In this study an attempt is made to differentiate the metals in the sediment into exchangeable, reducible and resistant fractions in the sediments.
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The present study is an attempt to address issues related to sediment properties like texture, mineralogy and geochemistry as well as water quality of two important rivers of central Kerala-the Periyar and the Chalakudy rivers. The main objectives of the study are to investigate the textural and mineralogical characteristics as well as transportation and depositional mechanisms of the sediments of Periyar and Chalakudy rivers, to find out the geochemical variability of organic carbon, phosphorus and certain major (Na,K,Ca and Mg) and minor/trace(Mn,Pb,Ni,Cr, and Zn) elements in the bulk sediments and mud fraction of these rivers, to evaluate the status of heavy metal pollution registered in the sediments of these rivers, to assess the physico-chemical characteristics and water quality of Periyar and Chalakudy rivers and to estimate the dissolved nutrient flux through the Periyar and Chalakudy rivers into the receiving coastal waters. The granulometric characteristics as well as statistical parameters of the sediments of Periyar and Chalakudy rivers depend on the flow pattern controlled by the gradient of the terrain. Compared to Periyar, fluctuations in the dispersal of particles are more in Chalakudy river. In Periyar river, the P and Fe in bulk sediments show a positive correlation with C-org, while in Chalakudy river, both the elements are related to THM concentration. In general, C-org, Fe and P Shows an increasing trend downstream. In Periyar river, the P and Fe in bulk sediments show a positive correlation with C-org, while in Chalakudy river, both the elements are related to THM concentration. Among these two rivers, the pollution of water is several fold higher in Periyar river due to influx due to influx of considerable quantity of liquid and solid wastes of industrial/domestic/urban origin. Nutrient analysis reveals 2-3 times increase in N and P during monsoon season whereas SiO2-Si shows a decreasing trend.
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The study deals with structural and spectral investigations of transition metal complexes of di-2-pyridyl ketone N(4),N(4)-disubstituted thiosemicarbazones. The main objective and scope of the work deals with di-2-pyridyl ketone N(4),N(4)-disubstituted thiosemicarbazones are quardridentate NNNS donor ligands. To chosen this ligand for study because, the ligands are prepared and characterized for the first time, since there are two pyridyl nitorgens, dimmers and polymers of complexes may result leading to interesting structural aspects. The work includes the preparation of the thiosemicarbzones and their structural and spectral studies, synthesis and spectral characterization of complexes of copper(II),,nickel(II),manganese(II), dioxovanadium(V),cobalt(III),zinc(II),cadmium(II) of the ligand HL, synthesis and spectral characterization of complexes of copper(II),manganese(II), of the ligand HL and the development of X-ray quality crystals and its X-ray diffraction studies. The structural characterization techniques are elemental analysis, conductivity measurements, magnetic measurements, electronic spectroscopy, H NMR spectroscopy, Infrared spectroscopy and X-ray crystallography.
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Solid phase extraction (SPE) is a powerful technique for preconcentration/removal or separation of trace and ultra trace amounts of toxic and nutrient elements. SPE effectively simplifies the labour intensive sample preparation, increase its reliability and eliminate the clean up step by using more selective extraction procedures. The synthesis of sorbents with a simplified procedure and diminution of the risks of errors shows the interest in the areas of environmental monitoring, geochemical exploration, food, agricultural, pharmaceutical, biochemical industry and high purity metal designing, etc. There is no universal SPE method because the sample pretreatment depends strongly on the analytical demand. But there is always an increasing demand for more sensitive, selective, rapid and reliable analytical procedures. Among the various materials, chelate modified naphthalene, activated carbon and chelate functionalized highly cross linked polymers are most important. In the biological and environmental field, large numbers of samples are to be analysed within a short span of time. Hence, online flow injection methods are preferred as they allow extraction, separation, identification and quantification of many numbers of analytes. The flow injection online preconcentration flame AAS procedure developed allows the determination of as low as 0.1 µg/l of nickel in soil and cobalt in human hair samples. The developed procedure is precise and rapid and allows the analysis of 30 samples per hour with a loading time of 60 s. The online FI manifold used in the present study permits high sampling, loading rates and thus resulting in higher preconcentration/enrichment factors of -725 and 600 for cobalt and nickel respectively with a 1 min preconcentration time compared to conventional FAAS signal. These enrichment factors are far superior to hitherto developed on line preconcentration procedures for inorganics. The instrumentation adopted in the present study allows much simpler equipment and low maintenance costs compared to costlier ICP-AES or ICP-MS instruments.
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In this regard Schiff base complexes have attracted wide attention. Furthermore, such complexes are found to play important role in analytical chemistry, organic synthesis, metallurgy, refining of metals, electroplating and photography. Many Schiff base complexes are reported in literature. Their properties depend on the nature of the metal ion as well as on the nature of the ligand. By altering the ligands it is possible to obtain desired electronic environment around the metal ion. Thus there is a continuing interest in the synthesis of simple and zeolite encapsulated Schiff base complexes of metal ions. Zeolites have a number of striking structural similarities to the protein portion of natural enzymes. Zeolite based catalysts are known for their remarkable ability of mimicking the chemistry of biological systems. In view of the importance of catalysts in all the areas of modern chemical industries, an effort has been made to synthesize some simple Schiff base complexes, heterogenize them by encapsulating within the supercages of zeoliteY cavities and to study their applications. The thesis deals with studies on the synthesis and characterization of some simple and zeoliteY encapsulated Mn(II), Fe(III), Co(II), Ni(II) and Cu(II) complexes and on the catalytic activity of these complexes on some oxidation reactions. Simple complexes were prepared from the Schiff base ligands SBT derived from 2-aminobenzothiazole and salicylaldehyde and the ligand VBT derived from 2-aminobenzothiazole and vanillin (4-hydroxy-3- methoxybenzaldehyde). ZeoliteY encapsulated Mn(II), Fe(III), Co(II), Ni(II) and Cu(II) complexes of Schiff base ligands SBT and VBT and also of 2-aminobenzothiazole were synthesized. All the prepared complexes were characterized using the physico-chemical techniques such as chemical analysis (employing AAS and CHN analyses), magnetic moment studies, conductance measurements and electronic and FTIR spectra. EPR spectra of the Cu(II) complexes were also carried out to know the probable structures and nature of Cu(II) complexes. Thermogravimetric analyses were carried out to obtain the information regarding the thermal stability of various complexes. The successful encapsulations of the complexes within the cavities of zeoliteY were ascertained by XRD, surface area and pore volume analysis. Assignments of geometries of simple and zeoliteY encapsulated complexes are given in all the cases. Both simple and zeoliteY encapsulated complexes were screened for catalytic activity towards oxidation reactions such as decomposition of hydrogen peroxide, oxidation of benzaldehyde, benzyl alcohol, 1-propanol, 2-propanol and cyclohexanol.
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The present study has been initiated to unravel the distribution of trace metals and its geochemical behavior in the Indian EEZ of the Arabian Sea and Bay of Bengal. Trace metal accumulation in aquatic consumers is of interest to ecologists and environmentalists so as to understand the fate and effect of contaminants in the food web dynamics and the biogeochemical cycling of trace metals. It is well established that oceanic distribution of macronutrients such as nitrate, phosphate and silicate provide critical to biological growth and related geochemical processes. In this study it can be inferred, that there is a need for a better understanding of background informations on trace metal concentrations with respect to space and time and their fluctuations in the Arabian Sea and Bay of Bengal zooplankton. Without a sound knowledge on spatio-temporal fluctuations, it will be impossible to differentiate anthropogenic metal inputs from natural background concentrations with a routine biomonitoring programme. Fe, Cu, Zn, Cd & Pb showed a slight enrichment in zooplankton from the Arabian Sea during spring intermonsoon compared to intermonsoon fall. The relative enrichment of Fe, Cu & Zn in zooplankton from the Arabian Sea during intermonsoon spring than intermonsoon fall was due to favourable bioaccumulation factors of these elements during this season. Nevertheless this study can be looked upon as a starting point for further investigations on these biogeochemically important processes, which are vital in addressing the dynamics of productivity of waters.
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In this paper, we report the measurements of thermal diffusivity of nano Ag metal dispersed ceramic alumina matrix sintered at different temperatures using laser induced non-destructive photoacoustic technique. Measurements of thermal diffusivity also have been carried out on specimens with various concentration of nano metal. Analysis of the data is done on the basis of one-dimensional model of Rosencwaig and Gersho. The present measurements on the thermal diffusivity of nano metal dispersed ceramic alumina shows that porosity has a great influence on the heat transport and the thermal diffusivity value. The present analysis also shows that the inclusion of nano metal into ceramic matrix increases its interconnectivity and hence the thermal diffusivity value. The present study on the samples sintered at different temperature shows that the porosity of the ceramics varies considerably with the change in sintering temperature. The results are interpreted in terms of phonon assisted heat transfer mechanism and the exclusion of pores with the increase in sintering temperature.
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In this paper, we report the measurements of thermal diffusivity of nano Ag metal dispersed ceramic alumina matrix sintered at different temperatures using laser induced non-destructive photoacoustic technique. Measurements of thermal diffusivity also have been carried out on specimens with various concentration of nano metal. Analysis of the data is done on the basis of one-dimensional model of Rosencwaig and Gersho. The present measurements on the thermal diffusivity of nano metal dispersed ceramic alumina shows that porosity has a great influence on the heat transport and the thermal diffusivity value. The present analysis also shows that the inclusion of nano metal into ceramic matrix increases its interconnectivity and hence the thermal diffusivity value. The present study on the samples sintered at different temperature shows that the porosity of the ceramics varies considerably with the change in sintering temperature. The results are interpreted in terms of phonon assisted heat transfer mechanism and the exclusion of pores with the increase in sintering temperature
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In this paper, we report the measurements of thermal diffusivity of nano Ag metal dispersed ceramic alumina matrix sintered at different temperatures using laser induced non-destructive photoacoustic technique. Measurements of thermal diffusivity also have been carried out on specimens with various concentration of nano metal. Analysis of the data is done on the basis of one-dimensional model of Rosencwaig and Gersho. The present measurements on the thermal diffusivity of nano metal dispersed ceramic alumina shows that porosity has a great influence on the heat transport and the thermal diffusivity value. The present analysis also shows that the inclusion of nano metal into ceramic matrix increases its interconnectivity and hence the thermal diffusivity value. The present study on the samples sintered at different temperature shows that the porosity of the ceramics varies considerably with the change in sintering temperature. The results are interpreted in terms of phonon assisted heat transfer mechanism and the exclusion of pores with the increase in sintering temperature
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Surface acidity of phosphate modified La2O3,CeO2 and SnO2 has been estimated by titrimetric Method using Hammett Indicators.Mixed Oxides of tin and lanthanum have also been prepared and subjected to phosphate modification.Surface characterizartion of the samples has been carried out using XRD, surface area,thermal analysis and IR spectroscopy. Phosphate content in the samples has been chemically estimated. The catalytic activity for benzylation and esterification reaction has also been investigated.
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The effect of residual cations in rare earth metal modified faujasite–Y zeolite has been monitored using magic angle spinning NMR spectral analysis and catalytic activity studies. The second metal ions being used are Na+, K+ and Mg+. From a comparison of the spectra of different samples, it is concluded that potassium and magnesium exchange causes a greater downfield shift in the 29Si NMR peaks. Also, lanthanum exchanged samples show migration behavior from large cages to small cages, which causes the redistribution of second counter cations. It is also observed that Mg2+ causes the most effective migration of lanthanum ions due to its greater charge. The prepared systems were effectively employed for the alkylation of benzene with 1-octene in the vapor phase. From the deactivation studies it is observed that the as-exchanged zeolites possess better stability towards reaction condition over the pure HFAU zeolite.
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To ensure quality of machined products at minimum machining costs and maximum machining effectiveness, it is very important to select optimum parameters when metal cutting machine tools are employed. Traditionally, the experience of the operator plays a major role in the selection of optimum metal cutting conditions. However, attaining optimum values each time by even a skilled operator is difficult. The non-linear nature of the machining process has compelled engineers to search for more effective methods to attain optimization. The design objective preceding most engineering design activities is simply to minimize the cost of production or to maximize the production efficiency. The main aim of research work reported here is to build robust optimization algorithms by exploiting ideas that nature has to offer from its backyard and using it to solve real world optimization problems in manufacturing processes.In this thesis, after conducting an exhaustive literature review, several optimization techniques used in various manufacturing processes have been identified. The selection of optimal cutting parameters, like depth of cut, feed and speed is a very important issue for every machining process. Experiments have been designed using Taguchi technique and dry turning of SS420 has been performed on Kirlosker turn master 35 lathe. Analysis using S/N and ANOVA were performed to find the optimum level and percentage of contribution of each parameter. By using S/N analysis the optimum machining parameters from the experimentation is obtained.Optimization algorithms begin with one or more design solutions supplied by the user and then iteratively check new design solutions, relative search spaces in order to achieve the true optimum solution. A mathematical model has been developed using response surface analysis for surface roughness and the model was validated using published results from literature.Methodologies in optimization such as Simulated annealing (SA), Particle Swarm Optimization (PSO), Conventional Genetic Algorithm (CGA) and Improved Genetic Algorithm (IGA) are applied to optimize machining parameters while dry turning of SS420 material. All the above algorithms were tested for their efficiency, robustness and accuracy and observe how they often outperform conventional optimization method applied to difficult real world problems. The SA, PSO, CGA and IGA codes were developed using MATLAB. For each evolutionary algorithmic method, optimum cutting conditions are provided to achieve better surface finish.The computational results using SA clearly demonstrated that the proposed solution procedure is quite capable in solving such complicated problems effectively and efficiently. Particle Swarm Optimization (PSO) is a relatively recent heuristic search method whose mechanics are inspired by the swarming or collaborative behavior of biological populations. From the results it has been observed that PSO provides better results and also more computationally efficient.Based on the results obtained using CGA and IGA for the optimization of machining process, the proposed IGA provides better results than the conventional GA. The improved genetic algorithm incorporating a stochastic crossover technique and an artificial initial population scheme is developed to provide a faster search mechanism. Finally, a comparison among these algorithms were made for the specific example of dry turning of SS 420 material and arriving at optimum machining parameters of feed, cutting speed, depth of cut and tool nose radius for minimum surface roughness as the criterion. To summarize, the research work fills in conspicuous gaps between research prototypes and industry requirements, by simulating evolutionary procedures seen in nature that optimize its own systems.
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Schiff base complexes of transition metal ions have played a significant role in coordination chemistry.In the present study we have synthesized some new Mn(II),Co(II) and Cu(II) complexes of Schiff bases derived from 1,8-diaminonaphthalene.Even though we could not isolate theses Schiff bases (as they readily cyclise to form the perimidine compounds),we were able to characterize unequivacally the complexes synthesized from these compounds as complexes of Schiff Bases. We Synthesized three perimidine derivatives ,2-(quinoxalin-2-yl)-2,3-dihydro-1H-perimidine,2-(2,3-dihydro-1H-perimidin-2-yl)-6-methoxyphenol and 4-(2,3-dihyro-1H-perimidin-2-yl)-2-methoxyphenol by the condensation of 1,8-diaminonaphthalene with quinoxaline-2-carboxaldehyde,2- hydroxy-3-methoxybenzaldehyde or 4-hydroxy-3-methoxybenzaldehyde respectively.Theses compounds were used as precursor ligands for the preparation of Schiff base complexes.The complexes were characterized by using elemental analysis ,conductance and magnetic susceptibility measuremets ,infrared and UV-Visible spectroscopy ,thermogravimetric analysis and EPR spectroscopy .We also encapsulated the complexes in zeolite Y matrix and these encapsulated complexes were also characterized. We have also tried theses complexes as catalysts in the oxidation of cyclohexanol and decomposition of hydrogen peroxide.