Abstract: A general procedure for the determination of the optimum instrumental parameters and the methods of sample preparation in qualitative and quantitative CMR analysis has been discussed. Four Couples of Solvent and relaxation regent are tried. The couple C₂D₂Cl₄/Fe(acac)₃ is the best. The minimum time of operation may be rebuced to about 1.0h and 4.0h for the qualitative and the qualitative analysis respectively for samples of medium molecular weight.