Abstract: A method for fast analysis of minimum hydrogen from mixture gas was established. This method was performed by using solid phase microextraction with a preparate Pd-5A molecule sieve, coated fiber coupled with gas chromatography. The results showed that the linear range of hydrogen was 0.001 1～0.125 0 mL/L. The limit detection is 9×10^-4 mL/L. This method compared to gas chromatography has the advantages of high sensitivity and less interference. The standard deviations of two methods are 8.7%.