Kß/Ka X ray intensity ratios from the electron capture decay of 51 Cr in S1 Cr (IH)-doped oxyanion salts were determined before and after annealing treatments. The observed change in the ratio is consistent with the overall process: 51 Cr (III) 51 Cr (VI), also inferred from solution analysis of the annealed samples. However, for most samples, the fraction of SI Cr (VI) calculated from the "in situ" analysis was less than that indicated by the solution analysis. No change in the ratio was seen with changes in the relative amounts of 51 Cr (III)-monomer and 51 Cr(III)-dimer + polymer. These observations suggest that the Kß/Ka "in situ" technique may be useful in following the overall process although it may not be sufficiently sensitive to distinguish the 51 Cr solid state precursor species.