Natural polymers like chitosan, hemp and man-made polymers like poly(ethylene oxide)(PEO) and hydroxypropyl methylcellulose (HPMC) were investigated using wide angle X-ray scattering (WAXS) method. The merits and demerits of natural and man-made polymers were quantified in terms of microcrystalline parameters, determined by whole powder pattern fitting technique, which is an extension of single order method developed by us.