The Pulsed Field Gradient (PFG) NMR spectroscopy was uesd to determine, via the diffusion coefficient, the molecular weights and the molecular weight distributions for sampels of poly(etylene glycol) (PEG) in D2O. Additional it was investigated, whether the components of mixtures of poly(ethylene glycol) with different molecular weights could be quantitatively determined by the differences in diffusion coefficient. The results of this study are compared with the result of the Dynamic Light Scattering (DLS) technique, the standard methode for the determination of molecular weights. The PFG NMR findings shows that the the molecular weights and the molecular weight distributions agreed well with values provided by the manufacturer. The mixtures could not be determined quantitativley, because of considerable overlaps in the molecular weight distributions. But it could be shown that the PFG NMR spectroscopy and the DLS technique complement one another.