A rapid and reliable method has been developed for the quantitative determination of sulphur in various geological samples with concentrations ranging from 50 mu g g(-1) to 4 wt % by using wavelength dispersive X-ray fluorescence spectrometry (WD-XRF). The samples were prepared as pressed pellets, and analysis was performed within a total measuring time of 20 seconds. The samples, prepared by the pressed pellet method, have an additional advantage in that the same pellet can be used for the determination of other major elements by XRF. A set of three international geochemical reference materials (GSR-6 GSR-5 and ASK-2) were,, used for calibration of the spectrometer. The accuracy of the data wa evaluated by analyzing 10 geochemical reference materials (ASK-1, ASK-2, FER-1, FER-2, GXR-1, CXR-3, GXR-4, NGRI-Au, GSR-5, GSR-6). The detection limit obtained for sulphur is adequate for several geochemical studies. The RSD <3 % and the limit of detection of 0.004 weight % obtained in this method suffice for the reliable estimation of sulphur in geological samples. A comparison was also made with the results obtained by another well-established method, e.g., a Leco Sulphur Analyzer, to reaffirm the suitability and accuracy of this method. A comparison of the results shows that the present methodology for the quantitative estimation of sulphur by WD-XRF is suitable for routine analysis in any geochemical laboratory with admissible accuracy and precision and can be used for geochemical exploration studies.
Laboratory experiments to probe the carbon dioxide sequestration potential of picritic basalts from the Deccan Basalt volcanic province, Maharashtra are reported. Growth of certain secondary carbonates is clearly seen over the surface of picritic basalts, reacted with water and carbon dioxide in its super-critical condition. The reactions were kept for about 5 months duration at a temperature and pressure of 100 degrees C and 60 bar of CO(2) respectively. Handpicked soft grains of secondary carbonates were characterized using infrared spectroscopy and the observed signatures in two of the picritic basalt samples (IGP-40 and IGP-29) match well with ankerite (Fe-carbonate), with negligibly small amounts of released SiO(2). While in another sample (IGP-36), the secondary carbonates have comparatively larger amounts of SiO(2).