A comparative study of sample dissolution techniques and plasma-based instruments for the precise and accurate quantification of REEs in mineral matrices

- Three types of digestion methods were tested.
- Four types of analytical techniques were compared.
- Elimination of the spectral interferences encountered in ICP-MS was achieved by the use of Tandem ICP-MS.
- Robustness of the analytical procedure was successfully evaluate on four types of certified reference material.

The recent commercialisation of inductively coupled plasma tandem mass spectrometric (ICP-MS/MS) instruments has provided analytical chemists with a new tool to properly quantify atomic composition in a variety of matrices with minimal sample preparation. In this article, we report on our assessment of the compatibility of 3 sample preparation techniques (open-vessel acid digestion, microwave digestion and alkaline fusion) for the quantification of rare earth elements (REEs) in mineral matrices. The combination of the high digestion temperatures (1050 °C) and using LiBO2 as a flux was the most effective strategy for the digestion of all rare earth elements in mineral matrices and was compatible with ICP-MS/MS measurements. We also assessed the analytical performances of ICP-MS/MS against other plasma-based instrumentation (microwave induced plasma and inductively coupled plasma atomic emission spectroscopy (MIP-AES and ICP-AES, respectively) and single quadrupole inductively coupled plasma mass spectrometry (ICP-MS). The comparative study showed that the concentrations obtained by ICP-MS/MS are in excellent agreement with the certified reference material values, and much more suited than the other analytical techniques tested for the quantification of REEs, which exhibited low detectability and/or spectral interferences for some elements/isotopes. Finally, the ruggedness of the analytical protocol proposed which combines a rapid sample dissolution step performed by an automated fusion unit and an ICP-MS/MS as a detector was established using various certified mineral matrices containing variable levels of REEs.

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