Abstract: Abstract: During the analyses of ore and rock samples by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS), many residues were formed in the tubes in which the hydride was generated, transport channelled and atomized. If a certain amount of the residues accumulat, they can distinctively affect the detection sensitivity of Se and Te. Many coexisting ingredients in the samples have a large influence on the detection of Se and Te by HG-AFS. In this article, to avoid interference from these ingredients, the series of standard solutions prepared with highly pure material were used. The standard solutions were tested with used tubes and cleaned ones. Through comparison of the data of the standard solutions, it was demonstrated that the residues in the instrument affected the detection of Se and Te by making the detection sensibility lower and the linear correlation coefficient smaller. The residues were analyzed with Atomic Fluorescence Spectrometry, Atomic Absorption Spectroscopy and Inductively Coupled Plasma-Atomic Emission Spectrometry. On the basis of the analytical results of the residues, Ti, Cu, As, Sb and Bi have great effect on the detection sensitivity and the linear correlation coefficient of Se and Te. These elements are a part of the coexisting interferences mentioned in literatures. When the tubes were cleaned, the measured quality was remarkably improved with higher sensitivity, and the linear correlation coefficient was more than 0.9995. According to the data obtained in this study, indications are that the analysis of residue components in the tubes is one of the effective methods to control the interference of HG-AFS.