OFFLINE AND ONLINE SOLID PHASE EXTRACTION/PRECONCENTRATION OF INORGANICS

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.

Unraveling a Benchmark for Sulphur Akin in the Cochin Estuarine System

The thesis deals with a benchmark study of dissolved and sedimentary sulphur compounds which play prominent roles in the prevailing redox conditions in the selected sites of Cochin estuarine system. Sulphur and its analogues play prominent roles in estuarine biochemical processes. A complete knowledge on the sulphur involvement in these processes is restricted due to the lacking of data on the organic sulphur compounds. Sulphate and sulphide in surface and bottom water and Sulphate, acid volatile sulphide and total sulphur in sediments were studied and correlated to know their interrelations in determining the redox condition of the environment. It also characterises the sediments of the sites on the basis of total organic carbon: total sulphur ratio. The study had attempted to decrease the concentration levels of sulphur in the sedimentary environment by the application of a remedial measure. Knowledge of sulphur uptake by plants from prior literatures has prompted to use phytoremediation for decreasing the sulphur concentration. Phytoremediation is an emerging technology that uses plants to clean up or remediate contaminated soil, sludges, sediments, and ground water through contaminant removal, degradation or containment. The plant selected was wheat grass since earlier studies have shown that wheat grass is effective in remediating pollutants particularly trace metals. So reduction in the concentration of selected trace metals was also focussed.