Microwave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductively coupled plasma-mass spectrometry

• Published in: Analytica chimica acta 2007-01, Vol.581 (2), p.247-259
• Main Authors: Kulkarni, Pranav, Chellam, Shankararaman, Mittlefehldt, David W.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Chemistry; Exact sciences and technology; Fluidized-bed catalytic cracking (FCC) catalysts; Inductively coupled plasma-mass spectrometry (ICP-MS); Instrumental neutron activation analysis (INAA); Lanthanides; Microwave digestion; Particulate matter (PM 2.5); Radiochemical methods; Rare earth elements; Spectrometric and optical methods
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2006.08.035

A robust microwave-assisted acid digestion procedure followed by inductively coupled plasma-mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM 2.5). High temperature (200 °C), high pressure (200 psig), acid digestion (HNO 3, HF and H 3BO 3) with 20 min dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst and PM 2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu and Dy in ambient PM 2.5 in an industrial area of Houston, TX.