Sealed capsules for convenient acquisition of variable-temperature controlled-atmosphere magic-angle-spinning NMR spectra of solids

1986 ◽  
Vol 68 (3) ◽  
pp. 561-563 ◽  
Author(s):  
T Adrian Carpenter ◽  
Jacek Klinowski ◽  
D Tilak ◽  
B Tennakoon ◽  
Cyril J Smith ◽  
...  
Keyword(s):  
Nmr Spectra ◽  
Variable Temperature ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Controlled Atmosphere ◽  
Temperature Controlled ◽  
Angle Spinning

Article

1999 ◽  
Vol 77 (11) ◽  
pp. 1962-1972
Author(s):  
Scott Kroeker ◽  
Roderick E Wasylishen
Keyword(s):  
Nmr Spectra ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Spin Coupling ◽  
Group Symmetry ◽  
Magic Angle ◽  
Chemical Shielding ◽  
Shielding Tensor ◽  
Angle Spinning ◽  
Spin Spin Coupling

Direct NMR observation of copper-63/65 nuclei in solid K3Cu(CN)4 provides the first experimental example of anisotropic copper chemical shielding. Axially symmetric by virtue of the space group symmetry, the shielding tensor spans 42 ppm, with the greatest shielding when the unique axis is perpendicular to the applied magnetic field. The nuclear quadrupole coupling constant is also appreciable, CQ(63Cu) = -1.125 MHz, reflecting a deviation of the Cu(CN)43- anion from pure tetrahedral symmetry. Spin-spin coupling to 13C nuclei in an isotopically enriched sample is quantified by line-shape simulations of both 13C and 63/65Cu magic-angle spinning (MAS) NMR spectra to be 300 Hz. It is shown that this information is also directly available by 63/65Cu triple-quantum (3Q) MAS NMR. The relative merits of these three approaches to characterizing spin-spin couplings involving half-integer quadrupolar nuclei are discussed. Chemical shielding tensors for nitrogen-15 and carbon-13 are obtained from NMR spectra of non-spinning samples, and are compared to those of tetrahedral group 12 tetracyanometallates. Finally, 2J(63/65Cu,15N) detected in 15N MAS experiments are found to be 19 and 20 Hz for the two crystallographically distinct cyanide ligands.Key words: NMR, quadrupolar nucleus, chemical shielding tensor, multiple-quantum magic-angle spinning, metal cyanide, spin-spin coupling.

Ultrafast high-resolution magic-angle-spinning NMR spectroscopy

The Analyst ◽  
2015 ◽  
Vol 140 (12) ◽  
pp. 3942-3946 ◽  
Author(s):  
Marion André ◽  
Martial Piotto ◽  
Stefano Caldarelli ◽  
Jean-Nicolas Dumez
Keyword(s):  
Nmr Spectroscopy ◽  
High Resolution ◽  
Nmr Spectra ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Magic Angle ◽  
Solid Samples ◽  
Semi Solid ◽  
Angle Spinning

The acquisition of ultrafast high-resolution magic-angle spinning (HR-MAS) NMR spectra of semi-solid samples is demonstrated.

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