Elemental analysis of atmospheric fine particles at trace and ultra-trace levels using microwave acid digestion and inductively coupled plasma - Mass spectrometry
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abstract
Quantitative recoveries (90-117%) for 20 certified and uncertified elements in a certified reference material of urban particulate matter (SRM 1648) validated that direct handling of hazardous HF during digestion of airborne particulate matter can be avoided by generating it in situ in closed Teflon-lined vessels by heating a mixture of NaF and HNO3. Two-stage sample digestion each with 20 min. dwell time, using HNO3 and NaF in the first stage and H3BO3 in the second stage with set points at 200C and 200 psig is recommended to assure the complete extraction of elements (other than Cr). Further, the method was optimized to accurately quantify 15 REEs and 27 non-REEs in petroleum refining FCC catalysts and atmospheric PM2.5. An addition of minimum but sufficient amount of HF and H3BO3 was crucial to analyze several REEs that are bound in aluminosilicate catalyst matrix. These methods provide robust protocols for the accurate and precise elemental analysis of urban particulate matter samples generated during air quality monitoring research that can be implemented in most laboratories.
