| OCR Text |
Show 1253.6 - (1165.96 + 74.7) = 12.94 then Charging energy constant (3) 1253.6 - 1195.35 - 12.94 = 45.31 or 45.3 Binding energy. (4) In the case of the second preliminary run, the alumina peak is 1167.69 and the arsenic peak is 1197.13; consequently the calculations are as follows: 1253.6 - (1167.69 + 74.7) = 11.21 Charging energy constant (5) 1253.6 - 1197.13 -11.21 = 45.26 or 45.3 Binding energy (6) The runs first documented the fact that ESCA could detect the arsenic in the flyash, and be used to determine its oxidation state. Both runs effectively document the presence of arsenic in the +5 state. It must be stressed, however, that these were preliminary runs and that it was assumed that the alumina peak was, in fact, an alumina peale. Internal spiking was not employed during these runs. 3.22. The Final Run Results Following the initial runs, a fmal run was made where the following procedure was employed: 1) internal standards for "pure" ASz03 and A~05 were developed and tested, and these standards were spiked with high concentrations of KCI; and 2) the flyash samples were spiked with high concentrations of KCI and then compared to internal standards; The results of this run are shown in Figs 3 and 4. From these tests, the CFee factor for the "pure" arsenic trioxide run was determined to be 11.78 and the charging factor for the "pure" arsenic pentoxide run was determined to be 10.61. The analysis of internal "pure" standards for arsenic trioxide and arsenic pentoxide then were calculated from measured peaks as follows : A~03 peak, 1198.21; ASzOs peak, 1197.25. The binding energy was then measured as follows: ASz03 ; 1253.6 - 11.78 - 1198.21 = 43.6 e V ASzOs = 1253.6 - 10.61 - 1197.25 = 45.7 eV (7) (8) These are within the regions shown in Table VITI, although the arsenic trioxide measurement is 0.2 eV below the lower range shown. The final ESCA run calculations on the flyash sample then produced calculated binding energies of 42.7 - 42.9 eV ash shown in Table IX. |
