Synchrotron radiation excited X-ray fluorescence analysis was utilized for characterization of trace impurities in synthetic diamonds. Advantage of the energy tunability was fully utilized to evaluate the attenuation of X-rays through the sample, and the absorption corrected X-ray fluorescence yield was utilized for quantitative analysis. Diamonds grown with several types of metallic solvents were investigated, and quantitative analysis of trace Co was carried out. It was found that Co prefers to be dissolved into (1 1 1) growth sector and that Co concentration in the (1 I 1) growth sector decreases one order of magnitude with the existence of Ni in the solvent. XANES spectra of dissolved Co shows characteristic pre-edge feature similar to that reported with the dissolved Ni. Experimental results suggest that both Ni and Co occupy in the similar site in the diamond lattice and that Ni is easier to be dissolved into diamonds.