Sequential automated fusion/extraction chromatography methodology for the dissolution of uranium in environmental samples for mass spectrometric determination

An improved methodology has been developed, based on dissolution by automated fusion followed by extraction chromatography for the detection and quantification of uranium in environmental matrices by mass spectrometry. A rapid fusion protocol (<8 min) was investigated for the complete dissolution of various samples. It could be preceded, if required, by an effective ashing procedure using the M4 fluxer and a newly designed platinum lid. Complete dissolution of the sample was observed and measured using standard reference materials (SRMs) and experimental data show no evidence of cross-contamination of crucibles when LiBO2/LiBr melts were used. The use of a M4 fusion unit also improved repeatability in sample preparation over muffle furnace fusion. Instrumental issues originating from the presence of high salt concentrations in the digestate after lithium metaborate fusion was also mitigated using an extraction chromatography (EXC) protocol aimed at removing lithium and interfering matrix constituants prior to the elution of uranium. The sequential methodology, which can be performed simultaneously on three samples, requires less than 20 min per sample for fusion and separation. It was successfully coupled to inductively coupled plasma mass spectrometry (ICP-MS) achieving detection limits below 100 pg kg−1 for 5-300 mg of sample.