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Sensitivity Considerations in Polarization Transfer and Filtering Using Dipole-Dipole Couplings: Implications for Biomineral Systems

Sensitivity Considerations in Polarization Transfer and Filtering Using Dipole-Dipole Couplings: Implications for Biomineral Systems

Sean C Christiansen, Niklas Hedin, Jan D Epping, Michael T Janicke, Yolanda del Amo, Mark Demarest, Mark Brzezinski, Bradley F Chmelka

Solid State Nucl Magn Reson. 2006 Feb;29(1-3):170-82.

PMID: 16343862

Abstract:

The robustness and sensitivities of different polarization-transfer methods that exploit heteronuclear dipole-dipole couplings are compared for a series of heterogeneous solid systems, including polycrystalline tetrakis(trimethylsilyl)silane (TKS), adamantane, a physical mixture of doubly (13)C,(15)N-enriched and singly (13)C-enriched polycrystalline glycine, and a powder sample of siliceous marine diatoms, Thalossiosira pseudonana. The methods were analyzed according to their respective frequency-matching spectra or resultant signal intensities. For a series of (13)C{(1)H} cross-polarization experiments, adiabatic passage Hartmann-Hahn cross-polarization (APHH-CP) was shown to have several advantages over other methods, including Hartmann-Hahn cross-polarization (HHCP), variable-amplitude cross-polarization (VACP), and ramped-amplitude cross-polarization (RACP). For X-Y systems, such as (13)C{(15)N}, high and comparable sensitivities were obtained by using APHH-CP with Lee-Goldburg decoupling or by using the transferred-echo double resonance (TEDOR) experiment. The findings were applied to multinuclear (1)H, (13)C, (15)N, and (29)Si CP MAS characterization of a powder diatom sample, a challenging inorganic-organic hybrid solid that places high demands on NMR signal sensitivity.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP4098980	Tetrakis(trimethylsilyl)silane		4098-98-0	Price

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