Abstract: The performance of anion solid phase extraction disk for the separation of TcO^-₄ ion in aqueous solution was studied systematically. The effects of flow rate, acidity, sample volume and soil matrix on adsorption were evaluated with different flow rate load conditions. And on this basis, an analysis procedure using solid phase extraction disk for the routine determination of ⁹⁹Tc in soil was presented. The procedure was validated by some simulated contaminated soil samples. The results show that ¹³⁷Cs, ⁹⁰Sr-⁹⁰Y, natural uranium and background radionuclides in soil do not interfere with the analysis procedure. The chemical yield of technetium is more than 95% for the whole procedure. The minimum detectable concentration is 1.1 Bq/kg with sample quantity of 10 g, background counting rate of 10 min^-1 and detection time of 10 h.