The simultaneous evaluation of all pH-dependent resonance signals (or multiplets) of an NMR titration offers a substantially increased accuracy and significance. The number of linearly independent titration equilibria is determined by graphical matrix rank analysis. The chemical shifts of all pH-dependent resonance l i e s are plotted against each other (chemical shift or CS diagrams) indicating whether a single or more titration equilibria are NMR spectrometrically observable and how far they overlap with each other. An iterative curve-fitting program allowing the simultaneous evaluation of all S@H) curves is available, from which pK vaIues and chemical shifts of all species can be calculated. The starting pK values for the iteration need only be estimated very approximately (accuracy &l-Z units). The titration end-points do not have to be experimentally accessible. The different methods for the simultaneous evalnation of all pH-dependent NMR signals are exemplified in the 31P NMR titration of thiamine pyrophosphate. In this case either the observed resonance lines (two doublets in a broad band proton decoupled spectrum) or the calculated chemical shifts for this AB system can be evaluated. A titration of sodium pyrophosphate was performed and evaluated for comparison.