39K quadrupole coupling and spin-lattice relaxation in the high temperature phases in KLiSO4

1990 ◽  
Vol 79 (2) ◽  
pp. 275-278 ◽  
Author(s):  
B. Topic ◽  
U. Haeberlen ◽  
R. Blinc
Keyword(s):  
High Temperature ◽  
Lattice Relaxation ◽  
Spin Lattice Relaxation ◽  
Spin Lattice ◽  
Quadrupole Coupling

Phase transitions in solid cycloheptene

1990 ◽  
Vol 68 (4) ◽  
pp. 604-611 ◽  
Author(s):  
Julian Haines ◽  
D. F. R. Gilson
Keyword(s):  
Phase Transition ◽  
High Temperature ◽  
Low Temperature ◽  
Lattice Relaxation ◽  
Proton Spin ◽  
Spin Lattice Relaxation ◽  
Temperature Phase ◽  
Scanning Calorimetry ◽  
Spin Lattice ◽  
Low Temperature Phase

The phase transition behaviour of cycloheptene has been investigated by differential scanning calorimetry, proton spin-lattice relaxation, and vibrational spectroscopy (infrared and Raman). Two solid–solid phase transitions were observed, at 154 and 210 K, with transition enthalpies and entropies of 5.28 and 0.71 kJ mol−1 and 34.3 and 3.4 JK−1, respectively. Cycloheptene melted at 217 K with an entropy of melting of 4.5 JK−1 mol−1. The bands in the vibrational spectra of the two high temperature phases were broad and featureless, characteristic of highly disordered phases. The presence of other conformers, in addition to the chair form, was indicated from bands in the spectra. The ring inversion mode was highly phase dependent and exhibited soft mode type behaviour prior to the transition from the low temperature phase. The low frequency Raman spectra (external modes) of these phases indicated that the molecules are undergoing isotropic reorientation. In the low temperature phase, the vibrational bands were narrow; the splitting of the fundamentals into two components and the presence of nine external modes are consistent with unit cell symmetry of either C2 or Cs with two molecules per primitive unit cell. A glassy state can be produced from the intermediate phase and the vibrational spectra were very similar to those of the high temperature phases, indicating that static disorder was present. The barriers to reorientation, as obtained from proton spin-lattice relaxation measurements, are 9.0 kJ mol−1 in both the high temperature phases, and 15.4 kJ mol−1 in the low temperature, ordered phase. Keywords: cycloheptene, phase transition, differential scanning calorimetry, NMR, vibrational spectroscopy.

17O Quadrupole Dips in Ammonium Persulphate

1994 ◽  
Vol 49 (1-2) ◽  
pp. 345-350 ◽  
Author(s):  
N. F. Peirson ◽  
J. A. S. Smith ◽  
D. Stephenson
Keyword(s):  
Relaxation Time ◽  
Lattice Relaxation ◽  
Quadrupole Coupling Constant ◽  
Lattice Relaxation Time ◽  
Spin Lattice Relaxation ◽  
Ammonium Persulphate ◽  
Spin Lattice Relaxation Time ◽  
Spin Lattice ◽  
Resonance Frequencies ◽  
Quadrupole Coupling

Abstract The magnetic field dependence of the 1H spin-lattice relaxation time in ammonium persulphate shows pronounced minima near the 1H magnetic resonance frequencies of 1,200 and 2,200 kHz. These are interpreted in terms of a model involving cross-relaxation between 1H in the NH4 ion and 17O in natural abundance in the S2O2-8 ions, the latter having a much shorter spin-lattice relaxation time. A theoretical analysis of the shape of the minima is used to derive values for the 17O quadrupole parameters. This analysis results in best estimate values for the quadrupole coupling constant of 6.75 (± 0.05) MHz and an asymmetry of 0.30 (± 0.02). Such values are indicative o f O-H hydrogen bonding and suggest the S2O2-8 ion is not undergoing rapid reorientation at temperatures below 320 K.

2 D Methods in NQR Spectroscopy

1992 ◽  
Vol 47 (1-2) ◽  
pp. 333-341
Author(s):  
J. Seliger ◽  
R. Blinc
Keyword(s):  
Double Resonance ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Electric Quadrupole ◽  
Quadrupole Coupling Constant ◽  
Spin Lattice Relaxation ◽  
Two Dimensional ◽  
Spin Lattice ◽  
Quadrupole Coupling ◽  
Field Cycling

AbstractThe application of two-dimensional spectroscopy to nuclear quadrupole resonance (NQR) is reviewed with special emphasys on spin 3/2 nuclei. A new two-dimensional level crossing double resonance NQR nutation technique based on magnetic field cycling is described. This technique allows for a determination of both the electric quadrupole coupling constant and the asymmetry parameter for spin 3/2 nuclei in powdered samples even in cases where the quadrupolar signals are too weak to be observed directly. It works if the usual double resonance conditions are met, i.e. if the spin-lattice relaxation times are not too short if the quadrupolar nuclei are dipolarly coupled to "strong" nuclei. Variations of this techique can be also used for 2 D "exchange" NQR spectroscopy and NQR imaging.

Structural Phase Transitions and Ionic Motions in Pyridinium Hexachlorotellurate(IV),Hexachlorostannate(IV), and Hexabromostannate(IV) Crystals as Studied by 1H NMR

1989 ◽  
Vol 44 (4) ◽  
pp. 300-306 ◽  
Author(s):  
Yutaka Tai ◽  
Tetsuo Asaji ◽  
Ryuichi Ikeda ◽  
Daiyu Nakamura
Keyword(s):  
Phase Transitions ◽  
High Temperature ◽  
Structural Phase ◽  
Lattice Relaxation ◽  
Relaxation Mechanism ◽  
Lattice Relaxation Time ◽  
Spin Lattice Relaxation ◽  
Scanning Calorimetry ◽  
Spin Lattice ◽  
H Nmr

Abstract The 1H NMR second moment M2 and the spin-lattice relaxation time T1 are determined for pyridinium hexachlorotellurate(IV), hexachlorostannate(IV), and hexabromostannate(IV) at various temperatures above ca. 140 K. The phase transition temperatures already reported from halogen NQR experiments are determined as 272, 331, and 285 K, respectively, by differential thermal analysis (DTA). The DTA as well as differential scanning calorimetry measurements show that the above phase transitions are of second-order. For pyridinium hexachlorotellurate(IV) and hexa-bromostannate(I V), a sharp 1H T1 dip was observed at the transition temperature. This is interpreted in terms of a phenomenon related to the critical fluctuation of an order parameter. From the measurements of 1H M2, 60° two-site jumps (60° flips) around the pseudo C6 axis of the cation are suggested to occur in the high temperature phases of the complexes. Modulation of X...1H (X = CI, Br) magnetic dipolar interactions due to the reorientational motion of the complex anions is considered as a possible relaxation mechanism in the high temperature phases.

Sign in / Sign up

Export Citation Format

Share Document