Abstract: Quality control procedures used for the determination of trace elements in fuel oil and coal are described. Two standard reference materials (NIST 1632a and 1632b) were used to evaluate the accuracy in the determination of As, Hg and Se in coal by flow injection (FI) hydride-generation (HG) AAS and FI HG ICP-MS after microwave solubilization (Anal. Chim. Acta, 1989, 225, 159). RSD over 2 years were 10% for As, 8.11% for Se and 15% for Hg. The use of real fuel oil samples to compare results obtained for the determination of Ni and V by NAA, ICP-MS, ETAAS and ICP-AES in 54 laboratories is discussed. Similarly, the use of real samples to detect significant bias in the determination of As, Hg and Se in coal using various techniques (NAA, FI HG AAS, FI HG ICP-MS, ETAAS) is discussed.

Abstract: Particulate matter in stack effluents of coal-fired plants was collected with an isokinetic probe nozzle suitable for (a) total particulate samplings on membrane filters and (b) sampling with a low volume 10-stage single orifice cascade impactor plus a backup filter. A microwave digestion method using an acid mixture of HNO3-HCl-HF in a closed vessel was developed for the determination of major, minor, and trace elements in very small amounts of sample. Analyses were carried out by inductively coupled plasma mass spectrometry (ICP-MS). A recovery study was conducted using multielemental standard solutions, NIST1633a Trace Elements in Coal Fly Ash and NIST 1648 Urban Particulate Matter, to examine the capabilities of the method. The results for real samples dissolved by this procedure were compared with results obtained by instrumental neutron activation anal., graphite furnace atomic absorption spectrometry, and flow injection hydride generation atomic absorption spectrometry. The anal. capabilities of ICP-MS make it one of the techniques of choice for the determination of trace elements in emission particulate matter collected in different granulometric particle sizes.