A method which is useful for a refined analysis of the highhyphen;resolution NMR spectra is presented. The method is based on the method of least squares. Before refinement of molecular constants, it is necessary to make a rough assignment of multiplet lines in a spectrum. Then the spectrum will be analyzed systematically with high precision. The ways to find a rough assignment are also discussed briefly. Although the method is applicable to any spin system, examples of analysis are shown by the spectra of three spin systems, the vinyl protons of acrylic acid, ethyl acrylate, and vinyl sulfonic acid. From these results, the method appears to be suitable for an analysis of the spectrum which is composed of superposed lines.
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