In the absence of a certified reference material, 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 (PM2.5). High temperature (200 °C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. 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 https://ntrs.nasa.gov/search.jsp? R=20060022633 2018-05-10T22:17:43+00:00Z 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 PM2.5 in an industrial area of Houston, TX. Analytical novelty of the research. We have developed and quantitatively verified microwave digestion and inductively coupled plasma -mass spectrometry techniques to accurately and precisely measure all naturally occurring rare earth elements in the aluminosilicate matrices of fluidized-bed catalytic cracking catalysts and atmospheric fine particles. One important basis of our research is that to date, no certified reference material is available for these zeolite-based catalysts. Additionally, existing reference materials for atmospheric particles such as SRM 1648 from the National institute of Standards and technology only include four rare earths (La, Ce, Sm, and Eu) and that too only as uncertified elements. were detected in PM 2.5 samples from Houston's Ship Channel area. We demonstrate that the loss of FCC catalyst from the refinery was the primary source of REEs in ambient atmospheric fine particles and that increase in PM 2.5 mass was predominantly caused by the loss of FCC catalyst during the "upset" event.
U N I V E R S I T Y of H O U S T O NI appreciate the opportunity to publish in Analytica Chimica Acta. As the corresponding author, please contact me at chellam@uh.edu if I can provide additional information.Sincerely,
Shankar Chellam Associate Professor Department of Civil and Environmental Engineering Department of Chemical EngineeringMicrowave-assisted extraction of rare earth elements from petroleum refining catalysts and ambient fine aerosols prior to inductive...