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information on molecular size and chemical composition in cases where multidetector setups are used. Multiple detection, however,is very complex. Using 1HNMRas the soledetector offers a number of significant benefits.First,NMRreplacestheneedtouse multidetector setups. Second, the structure and the microstructure of the molecules as well as the chemical composition of the molecules can be recorded. As the consequence, selective and

quantitative information can be directly obtained from the NMR chromatograms. Third, the molar mass distributions of all

separated species can be derived directly from these NMR chromatograms. The new online ThFFF−NMR coupling was successfully applied to homopolymers and block copolymers of different molar masses and chemical compositions