The EXAFS spectroscopy equipment constructed from an asymmetrical cut flat monochromator and PSPC is applied to the structural determination of pure α-iron which has small difference (0.038nm) in the first and second nearest neighbour distance. The efficiency of the curve fitting method for the two shell model of known structure material (α-iron) is discussed, in addition to describing the details of the experimental procedure of our new type of spectrometer and of the EXAFS data analysis.