Abstract: The Weihe basin has a good prospect of helium resources, so the determination of helium content is very important in exploration and investigation. In this paper, the determination method and application of He-Ne-H₂ in headspace samples from Weihe basin are studied. In this method, the water vapor contained in the sample and gas escape in the process of injection can be solved by air tight injection device. This improvement can improve the accuracy and stability of the results. The technology of valve switching back blowing is used to avoid interference of irrelevant components and protect chromatographic column. The analytical conditions were optimized by several experiments:carrier gas flow rate was 14 mL/min; TCD temperature was 180℃; Oven temperature was 40℃; Valve switching time was 0.65 min. The reliability of the method is determined by the detection limit, accuracy and precision. Finally, the method is applied to the measurement of helium in a headair sample in Weihe basin with satisfactory results. It is proved that this method has a good application prospect.