Styroflex/polyaniline (STF/PAni) blends were prepared by two routes namely by in situ and thermo mechanical processing method with various PAni compositions, namely, 0, 15, 30, and 45 wt %. The influence of volume fraction of PAni in the blends and synthetic routes of the STF/PAni blends on the volume resistivity and microcrystalline parameters have been investigated. The microcrystalline parameters such as the nanocrystal size (< N >), lattice disorder (g), interplanar distance (dhkl), width of the crystallite size distribution, surface weighted crystal size (Ds), and crystallite area were evaluated from the wide angle X-ray scattering profiles. The different asymmetric column length distribution functions namely, exponential, reinhold, and lognormal distribution methods were employed to probe the microcrystalline behavior of the STF/PAni blends and the results are compared. (c) 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011