Separation and measurement of Pa, Th, and U isotopes in marine sediments by microwave-assisted digestion and multiple collector inductively coupled plasma mass spectrometry.

This manuscript describes a new protocol for determination of Pa/Th/U in marine sediments. It is based on microwave-assisted digestion and represents an important reduction of working time over conventional hot-plate digestion methods, and the use of HClO(4) is avoided. Although Th and U are completely dissolved with a first microwave step, around 40% of (231)Pa remains undissolved, and a short hot-plate step with reverse aqua regia is required to achieve total digestion and spike equilibration. Next, the method involves a separation of these elements and a further purification of the Pa fraction using Dowex AG1-X8 resin. Separation with Bio-Rad and Sigma-Aldrich resins was compared; although both perform similarly for Th and U, Pa yields are higher with Bio-Rad. Finally, samples are measured using a Nu instruments multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS). Overall chemical yields range around 50% for Pa, 60% for Th, and 70% for U.