Abstract: Analytical methods for 25 cations. 5 anions, as well as total residue, total oxide, densily and free acid are developed. The HLLW sample taken from reprocessing plant was analysed by 18 different methods. Two or more methods with different principles are used to check the accuracy for the major chemical composition, and the obtained results are agreed well. The complete and accurate data are provided for further HLLW treatment and disposal.