• Journal of the Korean Chemical Society
• /
• v.68 no.2
• /
• pp.74-81
• /
• 2024

A sulfonic acid-water-silanol system in SO₃H-functionalized MCM-41 was investigated using solid-state nuclear magnetic resonance techniques. The proton exchange rate between a water molecule and a silanol group in the S-PE-MCM-41 was determined by analyzing the 1D proton spectra, the proton EXSY spectrum, and ²H spin-lattice relaxation data under various hydration levels. Two kinds of water-bounding sites were found in the S-PE-MCM-41: weakly and strongly bound sites. Over several hours, water molecules bound to the weakly bound sites at the low hydration level migrated to the strongly bound sites. At high temperature, the S-PE-MCM-41 easily lost water molecules weakly bound to the silanol, while the strongly bound water molecules survived. Water molecules that participated in the hydration of the phenethyl sulfonate were involved in the hydrogenbonded silanol mechanism of proton conductivity. This phenomenon contributes higher proton conductivity to the S-PE-MCM-41 by the cooperation of sulfonyl and silanol groups in the proton transfer process, even at higher temperature.

• Journal of the Korean Chemical Society
• /
• v.38 no.9
• /
• pp.628-631
• /
• 1994

We have studied the paramagnetic $CuF_2$ using the techniques of pulsed nuclear magnetic resonance (NMR). The powder sample revealed two well-separated lines from the distinct $^{19}F$ sites at room temperature. One of the lines showed little frequency shift. However, the other showed a large frequency shift, suggesting electron transfers. Furthermore, the two sites have very short spin-lattice relaxation times $(T_1).$ The frequency-shifted site has the shorter $T_1$ than the unshifted one, reflecting the difference of the electron environments of the two sites.

• Journal of the Korean Magnetics Society
• /
• v.5 no.3
• /
• pp.171-174
• /
• 1995

We have studied the paramagnetic $CuF_{2}$ using the techniques of pulsed nuclear magnetic resonance(NMR). The powder sample revealed two well-separated lines from the distinct $^{19}F$ sites at room temperature and at 77 K. The distinct frequency shifts of the two lines appear to arise from electron transfers. Furthermore, the two sites have very short spin-lattice relaxation times ($T_{1}$). The frequency-shifted site has the shorter $T_{1}$ than the unshifted one, reflecting the difference of the electron environments of the two sites.

• Journal of the Korean Magnetics Society
• /
• v.6 no.6
• /
• pp.397-404
• /
• 1996

The magnetic properties of $Ni_{1-x}Zn_{x}Fe_{2}O_{4}$ have been studied by X-ray diffractometry and $M\"{o}ssbauer$ Spectroscopy at room temperature. The X-ray diffraction study show that spinel structure is formed in all x, lattice constants linearly increased from $8.3111{$\AA$}~8.4184{$\AA$}({\pm}0.0003)$ with increasing x from 0 to 1, and oxygen parameter increase with increasing x. $M\"{o}ssbauer$ spectrum shows that $Ni_{1-x}Zn_{x}Fe_{2}O_{4}(x=0)$ has two antiparallel magnetic structure due to $Fe^{3+}$ octahedral site and $Fe^{3+}$ tetrahedral site. $Ni_{1-x}Zn_{x}Fe_{2}O_{4}$ with $0.2{\leq}x{\leq}0.6$ has magnetic structure of Yafet and Kittel, in particularly, specimen with x=0.6 shows relaxation effect. Specimen with $x{\geq}0.8$ show paramagnetic quadrupole splitting. The isomer shift is independent of x, but quadrupole splittings decrease with increasing x in the range of $0.8{\leq}x{\leq}1$, and nuclear magnetic fields decrease with in¬creasing x in the range of $0{\leq}x{\leq}0.6$. The magnetic properties of $Ni_{1-x}Zn_{x}Fe_{2}O_{4}$ change from ferrimagnetics to pararnagnetics with increasing x.

• Bulletin of the Korean Chemical Society
• /
• v.19 no.9
• /
• pp.934-942
• /
• 1998

$^13CO$ chemisorbed on platinum particles in L-zeolite has been investigated by static and magic angle spinning NMR spectroscopy. The representative spectra are composed of a broad asymmetric peak with a center of gravity at 230±30 ppm and a sharp symmetric peak at 124±2 ppm which is tentatively assigned to physisorbed $CO_2$, on inner walls of L-zeolite. Overall, the broad resonance component is similar to our previous results of highly dispersed (80-96%) CO/Pt/silica or CO/Pt/alumina samples, still showing metallic characters. The principal difference is in the first moment value. The broad peak in the spectra is assigned to CO linearly bound to Pt particles in the L-zeolites, and indicates a distribution of isotropic shifts from bonding site to bonding site. The NMR results reported here manifest that the Pt particles inside of the L-zeolites channels are not collectively the same with the ones supported on silica or alumina with similar dispersion in terms of Pt particle shape and/or ordering of Pt atoms in a particle. As a result, Pt particles of CO/Pt/L-zeolite were agglomerated accompanying CO desorption upon annealing. There were no definite changes in the NMR spectra due to differences of exchanged cations. Comparison of our observation on CO/Pt/L-zeolite with Sharma et al.'s reveals that even when the first moment, the linewidtb, and the relaxation times of the static spectra and the dispersion measured by chemisorption are similar, the properties of Pt particles can be dramatically different. Therefore, it is essential to take advantage of the strengths of several techniques together in order to interpret data reliably, especially for the highly dispersed samples.

• Geomechanics and Engineering
• /
• v.31 no.5
• /
• pp.519-527
• /
• 2022

Shear failure in soil is the primary cause of most geotechnical structure failures or instability. Soil water content is a significant factor affecting soil shear strength. In this study, the shear strength of samples with different water contents was tested. The shear strength, cohesion, and internal friction angle decreased with increasing water content. Based on the variation of cohesion and internal friction angle, the water content zone was divided into a high-water content zone and low-water content zone with a threshold water content of 15.05%. Cohesion and internal friction angle have a good linear relationship with water content in both zones. Environmental Scanning Electron Microscopy (ESEM) test presented that the aggregates size of the compacted loess gradually increases with increasing water content. Meanwhile, the clay in the compacted loess forms a matric that envelops around the surface of the aggregates and fills the inter-aggregates pores. A quantitative analysis of bound water and free water under different water contents using a nuclear magnetic resonance (NMR) test was carried out. The threshold water content between bound water and free water was slightly below the plastic limit, which is consistent with the results of shear strength parameters. Combined with the T2 distributions obtained by NMR, one can define a T2 relaxation time of 1.58 ms as the boundary point for bound water distribution without free water. Finally, the effects of bound water and free water on shear strength parameters were analyzed using linear regression analysis.

• Investigative Magnetic Resonance Imaging
• /
• v.8 no.2
• /
• pp.94-99
• /
• 2004

Purpose : To investigate the signal enhancement ratio by NOE effect on in vivo $^{31}P$ MRS in human heart muscle and liver. we also evaluated the enhancement ratios of different phosphorus metabolites, which are important in 31P MRS for each organ. Materials and Methods : Ten normal subjects (M:F = 8:2, age range = 24-32 yrs) were included for in vivo $^{31}P$ MRS measurements on a 1.5 T whole-body MRI/MRS system using $^1H-^{31}P$ dual tuned surface coil. Two-dimensional Chemical Shift Imaging (2D CSI) pulse sequence for $^{31}P$ MRS was employed in all $^{31}P$ MRS measurements. First, $^{31}P$ MRS performed without NOE effect and then the same 2D CSI data acquisitions were repeated with NOE effect. After postprocessing the MRS raw data in the time domain, the signal enhancements in percent were estimated from the major metabolites. Results : The calculated NOE enhancement for liver $^{31}P$ MRS were $\alpha-ATP\;(7\%),\;\beta-ATP\;(9\%),\;\gamma-ATP\;(17\%),\;Pi\;(1\%),\;PDE\;(19\%)$ and $PME\;(31\%)$. Because there is no creatine kinase activity in liver, PCr signal is absent. For cardiac $^{31}P$ MRS, whole body coil gave better scout images and thus better localization than surface coil. In $^{31}P$cardiac multi-voxel spectra, DPG signal increased from left to right according to the amount of blood included. The calculated enhancement for cardiac $^{31}P$ MRS were : $\alpha-ATP\;(12\%),\;\beta-ATP\;(19\%),\;\gamma-ATP\;(30\%),\;PCr\;(34\%),\;Pi\;(20\%),\;(PDE)\;(51\%),\;and\;DPG\;(72\%)$. Conclusion : Our results revealed that the NOE effect was more pronounced in heart muscle than in liver with different coupling to 1H spin system and thus different heteronuclear cross-relaxation.