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Microwave digestion-ICP-MS for elemental analysis in ambient airborne fine particulate matter: rare earth elements and validation using a filter borne fine particle certified reference material
Authors:Kulkarni Pranav  Chellam Shankararaman  Flanagan James B  Jayanty R K M
Affiliation:a Department of Civil and Environmental Engineering, University of Houston, Houston, TX 77204-4003, United States
b Department of Chemical and Biomolecular Engineering, University of Houston, Houston, TX 77204-4004, United States
c RTI International, Research Triangle Park, NC 27709, United States
Abstract:NIST standard reference material SRM 2783 was employed to validate a high temperature, high pressure, two-stage microwave assisted acid digestion procedure using HNO3, HF and H3BO3 developed for the analysis of trace elements (including rare earths) in atmospheric fine particulate matter (PM2.5) prior to inductively coupled plasma mass spectrometry (ICP-MS). This method quantitatively solubilized Na, Mg, Al, K, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sb, Cd, Cs, Ba, Pb, Th, U and several rare earth elements (REEs) (La, Ce, Pr, Nd, Gd, Dy, Er, Sm and Eu) from SRM 1648 and SRM 2783. A small amount of HF in the first stage was required to dissolve silicates necessitating the corresponding addition of H3BO3 in second stage to dissolve fluoride precipitates of Mg, La, Ce and Th. The optimized microwave dissolution—ICP-MS method detected Na, Mg, Al, K, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Cd, Mo, Sb, Cs, Ba, La, Ce, Pr, Nd, Sm, Gd, Pb, Th and U at trace to ultra-trace levels in ambient airborne fine particles from three sites in North Carolina. La to light lanthanide signature ratios suggested that soil and motor vehicles are the dominant REE sources in SRM 2783 and PM2.5 samples collected during this study.
Keywords:Inductively coupled plasma mass spectrometry (ICP-MS)   Microwave digestion   PM2.5   Standard reference material (SRM) 2783   Trace metals   Rare earth elements
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