scholarly journals Preparation, Thermal, and Physical Properties of Perovskite-Type (C3H7NH3)2CdCl4 Crystals

Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 108 ◽  
Author(s):  
Ae Lim ◽  
Sun Kim
Keyword(s):  
Phase Transitions ◽  
Physical Properties ◽  
Relaxation Times ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Scanning Calorimetry ◽  
Two Phase ◽  
Perovskite Type

To investigate the thermal and physical properties of perovskite-type (C3H7NH3)2CdCl4, its temperature-dependent chemical shifts and spin–lattice relaxation times are measured using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), magic angle spinning nuclear magnetic resonance (MAS NMR), and static NMR methods. Above 300 K, two phase transitions are observed at 398 K and 538 K. Each proton and carbon in the (C3H7NH3) cation is distinguished in the MAS NMR results. The environments around 1H, 13C, and 14N do not change with temperature according to the NMR spectra. In contrast, the resonance frequency of 113Cd in the CdCl6 octahedra decreases with increasing temperature, indicating an environmental change. The uniaxial rotations for 1H and 13C have high mobility at both high and low temperatures, and these are related to the phase transitions. In addition, the molecular motion of 113Cd in the anion becomes activated upon raising the temperature.

Application of High-Resolution-Magic-Angle-Spinning (HR-MAS) NMR Spectroscopy to Cosmetic Emulsions

2000 ◽  
Vol 55 (7) ◽  
pp. 651-656 ◽  
Author(s):  
Li-Hong Tseng ◽  
Detlef Emeis ◽  
Martin Raitza ◽  
Heidrun Händel ◽  
Klaus Albert
Keyword(s):  
Nmr Spectroscopy ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
2D Nmr ◽  
Magic Angle Spinning ◽  
Mas Nmr ◽  
Phase Changes ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Angle Spinning

Abstract HR-MAS NMR spectroscopy was utilized for the characterization of three cosmetic emul­sions. The emulsions had the same chemical composition and were prepared in the same way except the homogenization step. Magic angle spinning (M A S) of the emulsions was applied to improve signal resolution by eliminating susceptibility changes as well as residual dipolar interactions within the sample. Spin-lattice relaxation times (T1) were determined according to the inversion recovery technique in the temperature range of -10 °C to 40 °C to find out phase changes of the sample ingredients. 1H and 13C NMR signals of the individual components were assigned by use of different 1D and 2D NMR experiments. The HR-MAS NMR technique offers many possibilities to further investigate samples between the liquid and the solid state.

scholarly journals Study on Paramagnetic Interactions of (CH3NH3)2CoBr4 Hybrid Perovskites Based on Nuclear Magnetic Resonance (NMR) Relaxation Time

Molecules ◽  
2019 ◽  
Vol 24 (16) ◽  
pp. 2895 ◽  
Author(s):  
Ae Ran Lim ◽  
Sun Ha Kim
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Chemical Shifts ◽  
Relaxation Times ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Scanning Calorimetry ◽  
Paramagnetic Ions ◽  
Nuclear Magnetic

The thermal properties of organic–inorganic (CH3NH3)2CoBr4 crystals were investigated using differential scanning calorimetry and thermogravimetric analysis. The phase transition and partial decomposition temperatures were observed at 460 K and 572 K. Nuclear magnetic resonance (NMR) chemical shifts depend on the local field at the site of the resonating nucleus. In addition, temperature-dependent spin–lattice relaxation times (T1ρ) were measured using 1H and 13C magic angle spinning NMR to elucidate the paramagnetic interactions of the (CH3NH3)+ cations. The shortening of 1H and 13C T1ρ of the (CH3NH3)2CoBr4 crystals are due to the paramagnetic Co2+ effect. Moreover, the physical properties of (CH3NH3)2CoBr4 with paramagnetic ions and those of (CH3NH3)2CdBr4 without paramagnetic ions are reported and compared.

scholarly journals Physicochemical properties and structural dynamics of organic–inorganic hybrid [NH3(CH2)3NH3]ZnX4 (X = Cl and Br) crystals

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Ae Ran Lim ◽  
Sun Ha Kim ◽  
Yong Lak Joo
Keyword(s):  
Structural Dynamics ◽  
Chemical Shifts ◽  
Lattice Relaxation ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
Scanning Calorimetry ◽  
Inorganic Hybrid ◽  
Halogen Atoms

AbstractThe physical properties of the organic–inorganic hybrid crystals having the formula [NH3(CH2)3NH3]ZnX4 (X = Cl, Br) were investigated. The phase transition temperatures (TC; 268K for Cl and 272K for Br) of the two crystals bearing different halogen atoms in their skeletons were determined through differential scanning calorimetry. The thermodynamic properties of the two crystals were investigated through thermogravimetric analysis. The structural dynamics, particularly the role of the [NH3(CH2)3NH3] cation, were probed through 1H and 13C magic-angle spinning nuclear magnetic resonance spectroscopy as a function of temperature. The 1H and 13C NMR chemical shifts did not show any changes near TC. In addition, the 1H spin–lattice relaxation time (T1ρ) varied with temperature, whereas the 13C T1ρ values remained nearly constant at different temperatures. The T1ρ values of the atoms in [NH3(CH2)3NH3]ZnCl4 were higher than those in [NH3(CH2)3NH3]ZnBr4. The observed differences in the structural dynamics obtained from the chemical shifts and T1ρ values of the two compounds can be attributed to the differences in the bond lengths and halogen atoms. These findings can provide important insights or potential applications of these crystals.

Solid-state CP/MAS 13C NMR analysis of particle size and density fractions of a soil incubated with uniformly labeled 13C-glucose

Soil Research ◽  
1990 ◽  
Vol 28 (2) ◽  
pp. 193 ◽  
Author(s):  
JA Baldock ◽  
JM Oades ◽  
AM Vassallo ◽  
MA Wilson
Keyword(s):  
Solid State ◽  
Relaxation Times ◽  
Clay Fraction ◽  
Lattice Relaxation ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
Ultrasonic Probe ◽  
13C Nuclear Magnetic Resonance

A soil incubated for 34 days in the absence (control) and presence (treated) of uniformly labelled 13C-glucose was dispersed using an ultrasonic probe and fractionated by sedimentation in water and a polytungstate solution of density 2.0 Mg m3 . The residual substrate carbon was concentrated in the clay and light fractions. Solid state CP/MAS 13C n.m.r. (cross polarization/magic angle spinning 13c nuclear magnetic resonance) spectroscopy was used to characterize the chemical structure of the native soil organic carbon and the residual substrate carbon in the fractions of the control and treated soils. To obtain quantitative results it was essential to determine the spin lattice relaxation times in the rotating frame, T1pH, of the individual carbon types in the spectra as the relaxation behaviour of the native organic materials in the clay fraction was substantially different from that of the residual substrate carbon. After correcting for T1pH effects, a significant linear relationship existed between the signal intensity and 13C content of the samples. This enabled the content, expressed in �mol 13C g-1 fraction, of each type of carbon in the fractions to be calculated. The residual substrate carbon was found to accumulate in predominantly alkyl and O-alkyl structures in both fractions. However, significant amounts of acetal and carboxyl carbon were also observed in the clay fraction. Little if any aromatic or phenolic carbon was synthesized by the soil microorganisms utilizing substrate carbon. Dipolar dephasing CP/MAS 13C n.m.r. experiments were also performed and allowed the proportion of each type of carbon which was protonated and nonprotonated to be estimated. Essentially all of the O-alkyl and acetal carbon, 25-40% of the aromatic carbon and 66-80% of the alkyl carbon was protonated in the fractions isolated from the treated soil

scholarly journals Cation dynamics by 1H and 13C MAS NMR in hybrid organic–inorganic (CH3CH2NH3)2CuCl4

RSC Advances ◽  
2018 ◽  
Vol 8 (59) ◽  
pp. 34110-34115 ◽  
Author(s):  
Ae Ran Lim ◽  
Yong Lak Joo
Keyword(s):  
Chemical Shifts ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Mas Nmr ◽  
Spin Lattice Relaxation ◽  
Layered Perovskite ◽  
Spin Lattice ◽  
Nmr Techniques ◽  
Cp Mas Nmr ◽  
Perovskite Type

To understand the dynamics of the cation in layered perovskite-type (CH3CH2NH3)2CuCl4, the temperature-dependent chemical shifts and spin–lattice relaxation times T1ρ have been measured using 1H MAS NMR and 13C CP/MAS NMR techniques.

1H-Detected quadrupolar spin–lattice relaxation measurements under magic-angle spinning solid-state NMR

2019 ◽  
Vol 55 (39) ◽  
pp. 5643-5646 ◽  
Author(s):  
Maria Makrinich ◽  
Amir Goldbourt
Keyword(s):  
Solid State Nmr ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Proton Detection ◽  
Spin Lattice ◽  
Relaxation Measurements ◽  
Angle Spinning

Proton detection and phase-modulated pulse saturation enable the measurement of spin–lattice relaxation times of “invisible” quadrupolar nuclei with extensively large quadrupolar couplings.

scholarly journals Exploring the Role of Phosphate Structural Distortions on the Sodium Jump Dynamics in NASICON Phases

2015 ◽  
Vol 1773 ◽  
pp. 1-6
Author(s):  
Todd M. Alam ◽  
Nelson Bell ◽  
Jill Wheeler ◽  
Erik D. Spoerke ◽  
Randall T. Cygan ◽  
...  
Keyword(s):  
Sol Gel ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Spin Lattice ◽  
Relaxation Experiments ◽  
Jump Dynamics ◽  
Angle Spinning

ABSTRACTHigh temperature solid state sodium (23Na) magic angle spinning (MAS) NMR spin lattice relaxation times (T1) were evaluated for a series of NASICON (Na3Zr2PSi2O12) materials to directly determine Na jump rates. Simulations of the T1 temperature variations that incorporated distributions in Na jump activation energies, or distribution of jump rates, improved the agreement with experiment. The 23Na NMR T1 relaxation results revealed that distributions in the Na dynamics were present for all of the NASICON materials investigated here. The 23Na relaxation experiments also showed that small differences in material composition and/or changes in the processing conditions impacted the distributions in the Na dynamics. The extent of the distribution was related to the presence of a disordered or glassy phosphate phase present in these different sol-gel processed materials. The 23Na NMR T1 relaxation experiments are a powerful tool to directly probing Na jump dynamics and provide additional molecular level details that could impact transport phenomena.

scholarly journals Physicochemical Properties and Structural Dynamics of Organic–Inorganic Hybrid Perovskite [NH3(CH2)3NH3]ZnX4 (X=Cl and Br) Crystals

2021 ◽  
Author(s):  
Ae Ran Lim ◽  
Sun Ha Kim ◽  
Yong Lak Joo
Keyword(s):  
Structural Dynamics ◽  
Chemical Shifts ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Resonance Spectroscopy ◽  
Magic Angle ◽  
Scanning Calorimetry ◽  
Inorganic Hybrid ◽  
Halogen Atoms ◽  
Hybrid Perovskite

Abstract The physical properties of the organic–inorganic hybrid perovskite crystals having the formula [NH3(CH2)3NH3]ZnX4 (X=Cl and Br) were investigated. The phase transition temperatures (TC; 268 K for Cl and 272 K for Br) of the two crystals bearing different halogen atoms in their skeletons were determined through differential scanning calorimetry. The thermodynamic properties of the two crystals were investigated through thermogravimetric analysis. The structural dynamics, particularly the role of the [NH3(CH2)3NH3] cation, were probed through 1H and 13C magic-angle spinning nuclear magnetic resonance spectroscopy as a function of temperature. The 1H and 13C NMR chemical shifts did not show any changes near TC. In addition, the 1H spin-lattice relaxation time (T1ρ) varied with temperature, whereas the 13C T1ρ values remained nearly constant at different temperatures. The T1ρ values of the atoms in [NH3(CH2)3NH3]ZnCl4 were higher than those in [NH3(CH2)3NH3]ZnBr4. The observed differences in the structural dynamics obtained from the chemical shifts and T1ρ values of the two compounds can be attributed to the differences in the bond lengths and halogen atoms. These findings can provide important insights or potential applications of these crystals.

Molecular motion, phase transitions, and disorder in the pyridinium halides

1976 ◽  
Vol 54 (21) ◽  
pp. 3453-3457 ◽  
Author(s):  
John A. Ripmeester
Keyword(s):  
Phase Transitions ◽  
Molecular Motion ◽  
Relaxation Times ◽  
Lattice Relaxation ◽  
High Temperature Phase ◽  
Spin Lattice Relaxation ◽  
Temperature Phase ◽  
Pyridinium Chloride ◽  
Scanning Calorimetry ◽  
Spin Lattice

The solid pyridinium chloride, bromide, and iodide salts were studied using 1H nuclear magnetic resonance and differential scanning calorimetry. Phase transitions were observed at 345 K for the chloride, 269 K for the bromide, and 247 K for the iodide. Well below each transition, the pyridinium ions are held rigidly in the crystal lattice, whereas above each transition the ions reorientate rapidly about an axis at right angles to the ring planes. From the temperature dependence of the spin–lattice relaxation times the high temperature phase reorientational activation energies were determined to be 1.55, 2.30, and 4.20 kcal/mol for the chloride, bromide, and iodide, respectively.

Sign in / Sign up

Export Citation Format

Share Document