DETERMINATION OF THE TOTAL SULPHUR CONTENT OF OIL SHALE BY USING DIFFERENT ANALYTICAL METHODS

摘要

This paper presents the results of determination of the total sulphur content of Estonian and Chinese oil shales (OS) by using different analytical methods - elemental analysis, quantitative chemical analysis and X-ray fluorescence spectroscopy (XRF). The different forms of sulphur and respective quantities were determined in order to offer a possible explanation to the discrepancy between the results. Thermogravimetric analysis coupled with mass spectrometry (TGA-MS) was used as an additional tool to verify the release of SO2 and confirm the existence of sulphur in the organic and mineral parts of oil shale. Different analysis methods established different sulphur contents for the samples, showing a strong relationship between the sample composition and the analysis result. For both Estonian and Chinese oil shales the highest total sulphur content values, 1.53 and 2.23%, respectively, were determined using elemental analysis. As expected, the values were highly dependent on analysis conditions: the mass of sample and amount of catalyst used. The total sulphur contents of Estonian and Chinese oil shale samples as determined by the quantitative chemical analysis were 1.2 and 2.01%, respectively. Surprisingly, for Chinese oil shale the total sulphur content found by the quantitative chemical analysis was lower than that established by XRF. XRF determined the total sulphur contents of Estonian and Chinese oil shales to be 1.2 and 2.19%, respectively. These results suggest that elemental analysis should be the preferred method for the determination of total sulphur content.