Solid-State NMR of Elastomers

1990 ◽  
Vol 63 (3) ◽  
pp. 407-425 ◽  
Author(s):  
Robert A. Kinsey
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Variable Temperature ◽  
Heterogeneous Systems ◽  
Nmr Studies ◽  
High Magnetic Field Strength ◽  
Relaxation Measurements ◽  
Physical Insight ◽  
Elastomer Composites

Abstract The versatility of solid state NMR for the characterization of elastomers and elastomer composites has been demonstrated. NMR can be used as an analytical tool for identifying the elastomer(s) present (including the sequence distribution and tacticity), measuring crosslink levels, and monitoring chemical modifications. In addition, with relaxation measurements, NMR provides direct physical insight into the dynamics, and hence the spatial interactions of elastomeric systems. The interfacial regions of heterogeneous systems such as IPNs, filled elastomers, and block copolymers can be probed. A variety of NMR parameters can be correlated with physical properties. Future studies will extend the use of variable temperature and high magnetic field strength measurements, as well as utilize the growing number of two-dimensional experiments. The use of solid state H-l NMR should increase as instrumentation progresses, complementing the heteronuclear work. Solid H-l NMR offers significant sensitivity increases over C-13 NMR, but with decreased resolution. N-15 NMR studies have been recently performed at natural abundance with rigid polymers, and will likely be useful for characterizing elastomers.

Overexpression, purification, and characterization of recombinant Ca-ATPase regulators for high-resolution solution and solid-state NMR studies

2003 ◽  
Vol 30 (2) ◽  
pp. 253-261 ◽  
Author(s):  
Bethany Buck ◽  
Jamillah Zamoon ◽  
Tara L Kirby ◽  
Tara M DeSilva ◽  
Christine Karim ◽  
...  
Keyword(s):  
Solid State ◽  
High Resolution ◽  
Solid State Nmr ◽  
Purification And Characterization ◽  
Nmr Studies

Sol–gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

2016 ◽  
Vol 1119 ◽  
pp. 1-11 ◽  
Author(s):  
Simonas Kareiva ◽  
Vytautas Klimavicius ◽  
Aleksandr Momot ◽  
Jonas Kausteklis ◽  
Aleksandra Prichodko ◽  
...  
Keyword(s):  
Phase Composition ◽  
Solid State ◽  
Structural Characterization ◽  
Solid State Nmr ◽  
Sol Gel ◽  
Nmr Studies ◽  
Sol Gel Synthesis

Solution and Solid State NMR Studies of the Structure and Dynamics of C60 and C70

1990 ◽  
Vol 206 ◽  
Author(s):  
R. D. Johnson ◽  
C. S. Yannoni ◽  
J. Salem ◽  
G. Meijer ◽  
D. S. Bethune
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Variable Temperature ◽  
Chemical Shift Anisotropy ◽  
Resonance Assignments ◽  
Powder Pattern ◽  
High Symmetry ◽  
Nmr Studies ◽  
Structure And Dynamics ◽  
C Nmr

ABSTRACTWe have investigated the structure and dynamics of C60 and C70 with 13C NMR spectroscopy. In solution, high-resolution spectra reveal that C60 has a single resonance at 143 ppm, indicating a strained, aromatic system with high symmetry. This is strong evidence for a C60 “soccer ball” geometry. A 2D NMR INADEQUATE experiment on 13C-enriched C70 reveals the bonding connectivity to be a linear string, in firm support of the proposed “rugby ball” structure with D5h symmetry, and furnishes resonance assignments. Solid state NMR spectra of C60 at ambient temperatures yield a narrow resonance, indicative of rapid molecular reorientation. Variable temperature T1 measurements show that the rotational correlation time is ∼ 10−9s at 230 K. At 77 K, this time increases to more than 1 ms, and the 13C NMR spectrum of C60 is a powder pattern due to chemical shift anisotropy (tensor components 220, 186, 40 ppm). At intermediate temperatures a narrow peak is superimposed on the powder pattern, suggesting a distribution of barriers to molecular motion in the sample, or the presence of an additional phase in the solid state. A Carr-Purcell dipolar experiment on C60 in the solid state allows the first precise determination of the C60 bond lengths: 1.45 and 1.40Å.

scholarly journals Use of Solid-State NMR Spectroscopy for the Characterization of Molecular Structure and Dynamics in Solid Polymer and Hybrid Electrolytes

Polymers ◽  
2021 ◽  
Vol 13 (8) ◽  
pp. 1207
Author(s):  
Gabrielle Foran ◽  
Nina Verdier ◽  
David Lepage ◽  
Cédric Malveau ◽  
Nicolas Dupré ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Pulse Sequence ◽  
Dynamic Properties ◽  
Double Resonance ◽  
Solid Polymer ◽  
Pulse Field ◽  
Solid State Nmr Spectroscopy

Solid-state NMR spectroscopy is an established experimental technique which is used for the characterization of structural and dynamic properties of materials in their native state. Many types of solid-state NMR experiments have been used to characterize both lithium-based and sodium-based solid polymer and polymer–ceramic hybrid electrolyte materials. This review describes several solid-state NMR experiments that are commonly employed in the analysis of these systems: pulse field gradient NMR, electrophoretic NMR, variable temperature T1 relaxation, T2 relaxation and linewidth analysis, exchange spectroscopy, cross polarization, Rotational Echo Double Resonance, and isotope enrichment. In this review, each technique is introduced with a short description of the pulse sequence, and examples of experiments that have been performed in real solid-state polymer and/or hybrid electrolyte systems are provided. The results and conclusions of these experiments are discussed to inform readers of the strengths and weaknesses of each technique when applied to polymer and hybrid electrolyte systems. It is anticipated that this review may be used to aid in the selection of solid-state NMR experiments for the analysis of these systems.

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