In this paper, possible spin transformation and Co valence in dilute magnetic semiconductors is studied. Polycrystalline samples of Zn/sub 1-x/Co/sub x/O (0.05/spl les/x/spl les/0.17) and Zn/sub 1-z/Mg/sub z/Co/sub 0.15/O are prepared by rapid oxalate decomposition technique. X-ray diffraction is used to determine phase purity of the samples. Co valence state 2+ is determined by X-ray absorption near edge spectroscopy (XANES) using synchrotron irradiation. Magnetic properties measured show that all samples are paramagnetic and magnetization hysteresis measurement indicated that there is no trace of ferromagnetism. From Curie-Weiss fittings at high temperature region, the effective magnetic moment (/spl mu//sub eff/) is 3.87/spl mu//sub B//Co which corresponds to that of tetrahedral Co/sup 2+/ high spin state. When fitting at T approaches 0 K, /spl mu//sub eff/ = 2.82/spl mu//sub B//Co is observed indicating a possible spin state transition to Co/sup 2+/ low spin state.