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The implementation of direct standardization (DS), piecewise direct standardization (PDS), and double-window piecewise direct standardization (DWPDS) instrumental transfer techniques for high-resolution [sup.1]H NMR spectral data was explored. The ability to transfer a multivariate calibration model developed for a 'master or target' NMR instrument configuration to seven different ('secondary') NMR instrument configurations was measured. Partial least-squares (PLS) calibration of glucose, glycine, and citrate metabolite relative concentrations in model mixtures following mapping of the secondary instrumental configurations using DS, PDS, or DWPDS instrumental transfer allowed the performance of the different transfer methods to be assessed. Results from these studies suggest that DS and PDS transfer techniques produce similar improvements in the error of prediction compared to each other and provide a significant improvement over standard spectral preprocessing techniques including reference deconvolution and spectral binning. The DS instrumental transfer method produced the largest percent improvement in the predictions of concentrations for these model mixtures but, in general, required that additional transfer calibration standards be used. Limitations of the different instrumental transfer methods with respect to sample subset selection are also discussed.

Two-dimensional double quantum (DQ) [super 1]H MAS (magic angle spinning) NMR spectroscopy is used to investigate the dynamics of water environments in a series of polyoxoniobate alkali salts. The DQ [super 1]H MAS NMR studies have provided the chemical differences and variation in local water dynamics within materials without requiring isotopic substitution.