Proton solid-state nuclear

E. Vinogradov. P. K. Madhu and S. Vega, Proton spectroscopy in solid state nuclear magnetic resonance with windowed phase modulated Lee-Goldburg decoupling sequences. Chem. Phys. Lett., 2002, 354, 193-202. 

ER Andrew, M Kempka. Proton NMR study of molecular motion in solid cortisone. Solid State Nuclear Magn Reson 2 261-264, 1993. 

Solid-state nuclear magnetic resource (NMR) (proton and carbon)... 

See also Chromatography Overview. Liquid Chromatography Instrumentation Liquid Chromatography-Nuclear Magnetic Resonance Spectrometry. Nuciear Magnetic Resonance Spectroscopy Techniques Principles Multidimensional Proton Solid-State In Vivo Spectroscopy Using Localization Techniques. 

Overview Principles Instrumentation. Nuclear Magnetic Resonance Spectroscopy-Applicable Elements Fluorine-19 Nitrogen-15 Phosphorus-31 Organometallic Compounds. Nuclear Magnetic Resonance Spectroscopy Applications Food Pharmaceutical. Nuclear Magnetic Resonance Spectroscopy Techniques Nuclear Overha-user Effect Multidimensional Proton Solid-State. 

See also Nuclear Magnetic Resonance Spectroscopy Instrumentation. Nuclear Magnetic Resonance Spectroscopy Techniques Multidimensional Proton Solid-State. Peptides. 

Nuclear Overhauser Effect Multidimensional Proton Solid-State Surface Coil... 

FIGURE 2.97 H MAS NMR spectra of zeolites calcined at 433 K and dealnminated HY calcined at 673 K, rotor frequency was 10 kHz for 73LaNaY and 3 kHz for others. (Adapted from Solid State Nuclear Magn. Reson., 6, Hunger, M., Multinuclear solid-state NMR studies of acidic and non-acidic hydroxyl protons in zeolites, 1-29,1996, Copyright 1996, with permission from Elsevier.)... 

V. Sabarinathan, Z. Wu, R.-H. Chen, S. Ding, Multinuclear solid state nuclear magnetic resonance investigation of water penetration in proton exchange membrane NAFION 117 by mechanical spinning, J. Phys. Chem. B 117 (2013) 6558-6565. 

Ghassemzadeh, L., Marrony, M., Barrera, R., Kreuer, K. D., Maier, and Muller, K. 2009. Chemical degradation of proton conducting perfluorosulfonic acid ionomer membranes studied by solid-state nuclear magnetic resonance spectroscopy. Journal of Power Sources 186 334-338. 

Y. Pan, P- F rotational-echo double resonance nuclear magnetic resonance experiment on fluoridated hydroxyapatite. Solid State Nucl. Magn. Reson. 5 (1995) 263-268. L. Wu, W. Forsling, P.W. Schindler, Surface complexation of calcium mineral in aqueous solution, surface protonation at fluorapatite surface, J. Colloid Interface Sci. 147 (1991) 178-185. 

Solid-state C variable-amplitude cross polarization magic-angle spinning (VACP/MAS) nuclear magnetic resonance (NMR) spectra were acquired for the sorbitol samples. Proton decoupling was achieved by a two-pulse phase modulation (TPPM) sequence. Identical C spectra were measured for the y-form sorbitol samples, and a representative spectrum is shown in Figure 9. 

If high temperatures eventually lead to an almost equal population of the ground and excited states of spectroscopically active structure elements, their absorption and emission may be quite weak, particularly if relaxation processes between these states are slow. The spectroscopic methods covered in Table 16-1 are numerous and not equally suited for the study of solid state kinetics. The number of methods increases considerably if we include particle radiation (electrons, neutrons, protons, atoms, or ions). We note that the output radiation is not necessarily of the same type as the input radiation (e.g., in photoelectron spectroscopy). Therefore, we have to restrict this discussion to some relevant methods and examples which demonstrate the applicability of in-situ spectroscopy to kinetic investigations at high temperature. Let us begin with nuclear spectroscopies in which nuclear energy levels are probed. Later we will turn to those methods in which electronic states are involved (e.g., UV, VIS, and IR spectroscopies). 

The application of nuclear magnetic resonance (NMR) spectroscopy to polymer systems has contributed to significant advances in understanding of their structure and dynamical properties at the molecular level. From the analytical point of view, NMR spectroscopy is particularly suitable for a determination of the polymer structure by direct observation of the protons and carbons in different structural moieties. However, until the mid-1970s the application of this technique was limited to polymer solutions and to some elastomers in the solid state with a relatively high degree of the molecular mobility which allows the observation of the motionally narrowed absorption signals. 

Owing to the differences in both the nature and magnitude of the homo-and hetero-nuclear dipolar interactions, the process of eliminating the dipolar interactions to obtain a high resolution spectrum in the solid state is slightly different for protons and carbons, respectively, and will be reviewed separately in following... 

The 3-benzyl-6-phenyl-l,4-diazepine-2,5-diones 21 and 22 exhibited complex NMR spectra indicative of limited conformational mobility in which the ring geometry is dictated by the two air-amide elements, which define individual planes <2003MI187>. Based on an analysis of the nuclear Overhauser effect (NOE) between protons on the ring, the preferred boat conformation in solution projects the 3-benzyl moiety pseudoequatorially with the 6-phenyl substituent disposed axially or equatorially, dependent upon the relative stereochemistry. This conformation is also observed in the solid state for the air-substituted isomer 21 in which the phenyl group is axial. In contrast, the bis-phenyl derivative 23 is conformationally mobile based on the H NMR spectmm where resonances were not resolved. 

The solid state high resolution n.m.r. spectra were run on a CXP 200 BruKer spectrometer in which the 31P nucleus resonates at 81 MHz. Samples used were finely powedered and hand-tamped in glass tubes. The spectra were recorded using the Proton Enhanced Nuclear Induction Technique (6) on the same basis of a one shot cross polarization and high power decoupling during acquisition. A capillary tube of trimethylphosphate inserted in the powder sample is used as internal reference. 

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