Standard reference material and different geological samples were dissolved by system A (the mixture of nitric and perchloric acids) and system B (mixture of nitric, perchloric and hydrofluoric acids), and total Se in all samples was measured by hydride-generation atomic fluorescence spectrometry (HG-AFS) after concentration with thiol cotton fiber (TCF). The analytical results obtained by the two digestion method are in good agreement (within the limit of errors) for most of the samples, particularly for those having recommended values. The Se concentrations determined by the two methods are of no difference, and the correlation coefficient is 0.9986; the relative standard deviation (RSD) for the determination of 0.04 μg/g Se is 10.2%. The recovery rates of systems A and B by the stan- dard-addition method were 96%–106% and 99%–104%, respectively. Standard reference material and different geological samples were dissolved by system A (the mixture of nitric and perchloric acids) and system B (mixture of nitric, perchloric and hydrofluoric acids), and total Se in all samples was measured by hydride-generation atomic fluorescence spectrometry (HG-AFS) after concentration with thiol cotton fiber (TCF). The analytical results obtained by the two digestion method are in good agreement (within the limit of errors) for most of the samples, particularly for those having recommended values. The Se The determined rates of the systems A and B by the stan-dard are determined by the two methods are no difference, and the correlation coefficient is 0.9986; the relative standard deviation (RSD) for the determination of 0.04 μg / g Se is 10.2% dard-addition method were 96% -106% and 99% -104%, respectively.