HEEP COPYRIGHT: BIOL ABS. The coal sample is ashed with high temperature ashing or with RF plasma low temperature ashing. The coal ash or fly ash can be analyzed for major ash elements by fusing with lithium tetraborate in an automatic fusion device, the Claisse Fluxer. The ash samples are dissolved in a Parr bomb in a mixture of aqua regia and HF. The solutions are analyzed for 8 major (Al, Ca, Fe, K, Mg, Na, Si and Ti) and 20 trace elements (As, B, Ba, Be, Cd, Co, Cr, Cu, Li, Mn, Mo, Ni, P, Pb, Sb, Se, Sr, U, V and Zn) by inductively coupled plasma emission spectroscopy. Hg in coal and fly ash is determined on a separate aliquot by the cold vapor atomic absorption technique. F and Cl in the samples are determined by fusing with Na2CO3 and Eschka mixture, respectively, and then measuring the 2 ions in solution with specific ion electrodes. O2 in the samples can be determined rapidly and non-destructively by 14 MeV neutron activation analysis. These methods were tested by analyzing several NBS (National Bureau of Standards) coal and fly ash standards with good accuracy and reproducibility.