• 분석과학
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• 제12권3호
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• pp.184-189
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• 1999

수용액에서 vanadate와 N-benzyliminodiacetate (Bz-IDA) 리간드의 상호작용을 $^{51}V$ 핵자기공명분광법과 순환전압-전류법을 이용하여 조사하였다. $^{51}V$ 핵자기공명분광법 결과 바나듐(V)-Bz-IDA착물생성에 의한 두 개의 특정 피크(-515.5 ppm 및 -500.1 ppm)를 관찰할 수 있었다. 순환전압-전류법을 이용하여 얻어진 결과 바나듐(V)-Bz-IDA착물의 산화-환원파의 전위값은 각각 -0.05 V 및 -0.13 V에서 관찰하였다. 이로써 산화-환원반응은 가역적 일전자반응으로 추정되었다.

• 한국자기공명학회논문지
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• 제4권1호
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• pp.1-11
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• 2000

Supported vanadium oxides are being used extensively as catalysts for a variety of reactions, including partial oxidations and ammoxidations. A series of vanadium oxide supported on TiO2-ZrO2 was obtained by impregnating ammonium metavanadate slowly into a mixed precipitateof Ti(OH)4-Zr(OH)4, followed by calcining in air at high temperatures. The prepared catalysts were characterized by 51V solid-state NMR. In the calcined catalysts 51V NMR studies indicated the peaks corresponding to distorted tetrahedral vanadia species at low V2O5 contents and octahedral vanadia species at high vanadia loadings. These results illustrate the suitability of 51V NMR as a unique quantitative spectroscopic tool in the structural analysis of vanadium(V) oxide catalytic materials.

• Bulletin of the Korean Chemical Society
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• 제19권8호
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• pp.856-862
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• 1998

Vanadium oxide catalyst supported on ZrO2-WO3 was prepared by adding the Zr(OH)4 powder into a mixed aqueous solution of ammonium metavanadate and ammonium metatungstate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using solid-state 51V NMR and FTIR. In the case of calcination temperature at 773 K, for the samples containing low loading V2O5 below 18 wt % vanadium oxide was in a highly dispersed state, while for samples containing high loading V2O5 equal to or above 18 wt % vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of ZrO2-WO3. The ZrV2O7 compound was formed through the reaction Of V2O5 and ZrO2 at 873 K and the compound decomposed into V2O5 and ZrO2 at 1073 K, which were confirmed by FTIR and 51V NMR.

• 한국자기공명학회논문지
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• 제1권1호
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• pp.1-6
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• 1997

Several dioxovanadate (V) complexes are synthesized and studied by solution and solid-state 51V NMR spectroscopy. In the results, large 51V chemical shift anisotropy ({{{{ DELTA delta }}a = -800 ∼720 ppm) and quadrupole coupling (e2q /h = 7.50 ∼ 9.16 MHz) were observed in the solid-state complexes. The isotropic chemical shifts of the solid samples are very close to the values obtained from solution measurements.

• Bulletin of the Korean Chemical Society
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• 제21권9호
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• pp.913-918
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• 2000

Vanadium oxide catalyst supported on TiO2-ZrO2 has been prepared by adding Ti(OH)4-Zr(OH)4 powder to an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The char-acterization ofthe prepared catalysts was performed using solid-state 51V NMR and FTIR.In thecase ofcalci-nation temperature at 773 K, vanadium oxide was in a highly dispersed state for the samples containing low loading V2O5 below 25 wt %, but for samplescontaining high loading V2O5 equal to or above 25 wt %, vana-dium oxidewas well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2.The ZrV2O7 compound was formed through the reactionof V2O5 and ZrO2 at 773-973 K, where-as the V3Ti6O17 compound was formedthrough the reaction of V2O5 and TiO2 at 973-1073 K. The V3Ti6O17 compound decomposed to V2O5 and TiO2 at 1173 K, which were confirmed by FTIR and 51V NMR.

• Bulletin of the Korean Chemical Society
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• 제24권3호
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• pp.311-317
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• 2003

Vanadium oxides supported on zirconia and modified with MoO₃were prepared by adding Zr(OH)₄powder into a mixed aqueous solution of ammonium metavanadate and ammonium molybdate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using FTIR, Raman spectroscopy and solid-state $^{51}V$ NMR. In the case of a calcination temperature of 773 K, for samples containing low loading of $V_2O_5$, below 15 wt %, vanadium oxide was in a highly dispersed state, while for samples containing high loading of $V_2O_5$, equal to or above 15 wt %, vanadium oxide was well crystallized because the $V_2O_5$ loading exceeded the formation of a monolayer on the surface of $ZrO_2$. The $ZrV_2O_7$ compound was formed through the reaction of $V_2O_5\;and\;ZrO_2$ at 873 K and the compound decomposed into $V_2O_5\;and\;ZrO_2$ at 1073 K, which were confirmed by FTIR spectroscopy and solid-state $^{51}V$ NMR. IR spectroscopic studies of ammonia adsorbed on $V_2O_5-MoO_3/ZrO_2$ showed the presence of both Lewis and Bronsted acids.

• Bulletin of the Korean Chemical Society
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• 제25권1호
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• pp.106-108
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• 2004

In this paper we have determined the thermodynamic parameters for the isomerization between the ${\alpha}$-cis and the ${\beta}$-cis isomers in vanadium(V)-propylenediaminetetraacetate complex in water by $^{51}V$ NMR spectroscopy. In addition, the effects of organic solvents (methanol, formamide and dimethylsulfoxide) and inorganic salts (NaCl, $NaClO_4\;and\;NH_4Cl$) on the isomerization in solution have been investigated.

• Bulletin of the Korean Chemical Society
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• 제18권1호
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• pp.70-75
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• 1997

A wide range (10 < Si/V) of mesoporous vanadium silicate molecular sieves with the MCM-41 structure have been synthesized using vanadyl sulfate as the source of vanadium and characterized by XRD, 51V MAS NMR and 29Si MAS NMR. The increase of the unit cell parameter and the decrease of Q3/Q4 ratio of 29Si spectra with the vanadium content suggest the incorporation of vanadium in the framework of MCM-41 structure. 51V MAS NMR demonstrates that vanadiums in as-synthesized V-MCM-41 are present in the chemical environment of octahedra and octahedral vanadium is decreased and tetrahedral vanadium is increased inversely with raising the calcination temperature. Though the thermal treatment in rotor of hydrated sample resulted in the change from tetrahedral environment to octahedral one and the steaming and the acid treatment affect to the chemical environment of vanadium, the spectrum similar to originally calcined sample is regenerated after recalcination. This indicates that the vanadium is belong to the framework in a relatively exposed site. The best quality XRD pattern of the product of Si/V=27 may be attributable to heterogeneous nucleation mechanism. V-MCM-41's having the Si/V ratio lower than 20 are completely collapsed after calcination.

• 한국자기공명학회논문지
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• 제1권1호
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• pp.45-58
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• 1997

Heteropoly compounds, H3PMo12O40, CsxH3-xPMo12O40, and vanadium containing heteropoly compound were characterized by Solid-state broad line 1H MAS NMR, 31P MAS NMR, and High Speed MAS 51V NMR spectroscopy of quadrupolar nuclei. The effects of calcination, dehydration, and the number of protons on the structure of heteropoly compounds were studied. The results of this study demonstrate that these Solid-state NMR techniques are very useful tools to study heteropoly compounds.

• 대한화학회지
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• 제51권4호
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• pp.356-360
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• 2007

sodium ethoxide의 존재하에서 3,5-diaryl-cyclohex-2-en-1-one와 methyl vinyl ketone로부터 5,7-Diaryl- 3,4,6-trihydronaphthalen-2-ones가 합성되었다. 이 생성물은 IR, UV-Visible, 1H-NMR, 13C-NMR 그리고 mass spectral techniques로 구조를 규명하였다. 1H과 13C signals의 피크들은 HSQC spectrum을 찍어 정확히 규명하였다.