Determination of sulphur in uranium matrix by total reflection X-ray fluorescence spectrometry

作者：Dhara Sangita; Misra N L^*; Aggarwal S K

来源：Spectrochimica Acta Part B: Atomic Spectroscopy , 2008, 63(12): 1395-1398.

DOI：10.1016/j.sab.2008.10.033

• Total reflection X-ray fluorescence spectrometry
• Trace element
• Sulphur
• Uranium
• Solvent extraction

The possibility of sulphur determination in uranium matrix by total reflection x-ray fluorescence spectrometry (TXRF) has been studied. Calibration solutions and samples of sulphur in uranium matrix were prepared by mixing uranium in form of a standard uranyl nitrate solution and sulphur in the form of Na(2)SO(4) standard solution. prepared by dissolving Na(2)SO(4) in Milli-Q water. For major element analysis of sulphur, it was determined without separation of uranium whereas for the trace level determinations, uranium was first separated by solvent extraction using 30% tri-n-butyl phosphate (TBP) in dodecane as an extractant. In order to countercheck the TXRF results, a few samples of Rb(2)U(SO(4))(3), a chemical assay standard for uranium, were diluted to different dilutions and sulphur content in these solutions were determined. The TXRF determined results for trace determinations of sulphur in these diluted solutions were counterchecked after addition of another uranium solution, so that sulphur is at trace level compared to uranium, separating uranium from these solution mixtures using TBP extraction and determining sulphur in aqueous phase by TXRF. For such TXRF determinations, Co was used as internal standard and W L alpha was used as excitation source. The precision and accuracy of the method was assessed for trace and major element determinations and was found to be better than 8% (1 sigma RSD) and 15% at a concentration level of I mu g/mL of sulphur measured in solutions whereas for Rb(2)U(SO(4))(3), these values were found to be better than 4 and 13%, respectively.

• 出版日期2008-12