X-ray photoelectron spectroscopy(XPS) and extended X-ray absorption fine structure(EXAFS) were used to characterize the structure of the mixture of molybdenum oxide and anatase calcined at 723 K. The results indicate that molybdenum oxide can disperse onto the surface of anatase(TiO2) and the dispersion threshold is 11.2 mg in per gram of MoO3 or 4.8 Mo atoms/nm2 TiO2. When the content of MoO3 is below the dispersion threshold, MoO3 species is in highly dispersed state interacting strongly with TiO2 support and in discrete tetrahedral coordination, [MoO4], on the surface of TiO2. When the MoO3 loading is above this value, MoO3 exists in both dispersed phase and crystalline phase. MoO3 in dispersed phase is still a discrete [MoO4] tetrahedron; MoO3 in crystal phase is in octahedral coordination.
The reaction of palladium chloride with isovanillin semithiocarbazone (VSTC),CH3O(OH)C6H3CH=NNC(S)NH2, in a mixed solvent of ethanol, pyridine and water yielded the mononuclear palladium(Ⅱ) complex Pd[CH3O(O)C6H3CHNNC(S)NH2](C5H5N), and its singlecrystal structure was determined by X-ray diffraction. The crystal belongs to triclinic, space group P1-with a = 7.715(4), b = 9.809(6), c = 10.612(4) , α = 93.54(4), β = 111.00(3), γ= 95.92(5)°, V =745.0(7) A3, Mr= 408.75, Z = 2, Dc= 1.822 g/em3, t= 1.397 mm-1, and F(000) = 408. The final R =0.0568 and wR = 0.1439 for 2616 observed independent reflections with Ⅰ> 2.0σ(Ⅰ). It was revealed that the palladium atom is bound to a tridentate donor ligand and a pyfidine in a planar square arrangement. The sulphur-nitrogen-oxygen donor of the Schiff-base ligand in the thiol form rather than the thione one is coordinated to the palladium atom via the mercapto sulphur, the β-nitrogen and the hydroxylate oxygen atoms.
The monolayer dispersion of molybdenum oxide on the surface of alpha-Al2O3 has been studied by X-ray photoelectron spectroscopy (XPS) and extended X-ray absorption fine structure (EXAFS). The dispersion threshold is 4.65 mg MoO3 per g alpha-Al2O3 or 5.6 Mo atoms nm(-2). The structure of supported MoO3 is strongly dependent on the MoO3 loading. When the amount of MoO3 is below the dispersion threshold, the MoO3 species are highly dispersed on the surface of alpha-Al2O3, with the dispersed phase consisting of discrete [MoO4] polyhedrons. When the MoO3 loading exceeds the dispersion threshold, crystalline MoO3 appears on the surface of alpha-Al2O3. MoO3 exists in both dispersed and crystalline phases. According to the theory of phase isolation, the dispersed phase remains in the form of discrete [MoO4] polyhedrons. However, the crystalline phase of MoO3 is octahedral.
A new method for analysing the ingredients of Isrhynchophylline in Uncaria Rhynchophylla Jacks by thin layer chromatography (TLC) and the surface-enhanced Raman spectroscopy (SERS) is reported in this paper. The results show that the characteristic spectra bands of Isrhynchophylline situated at the thin layer with the amount of sample about 2.5 micrograms were obtained. The difference between SERS and solid spectra was found. Great enhancement of the 1,615 cm-1 spectral band was abstained. Molecule was absorbed in surface silver sol by pi electrons in phenyl and by pair of electrons in N together. An absorption model of Isrhynchophylline and silver sol was proposed. This method can be used to analyse the chemical ingredients with high sensitivity.
The co-precipitated ZnO/gamma-Al2O3 system calcined under 200degreesC, 300degreesC,450degreesC and 800 degreesC was studied here using XRD and EXAFS and the Zn-centered Radial Distribution Functions were obtained. The nearest Zn-O shell was fitted and a conclusion was drawn that the Zn is coordinated by 4 oxigen atoms, just like within the original ZnO crystal. The changing tendency of RDF peaks of the second Zn-centered shell with the ZnO loading was also discussed.
The reaction of tetraethylammonium metavanadate, (Et4N)VO3, with isovanillin semithiocarbazone(VSTC), HOC6H3(OCH3)CH=NNHCSNH2, in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate((V)) complex, [(C2H5)(4)N] [(VO2)-O-(V) (OC6H3(OCH3)CHNNCSNH2)].H2O (C17H31N4O5SV, M-r = 454.5) and its single-crystal structure has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group P2(1)2(1)2(1) with unit cell parameters a = 12.940(3), b= 15.414(3), c = 10.703(2) Angstrom, V= 2134.8(11) Angstrom (3), Z=4, D-calc 1.414 Kg/m(3), mu = 0.597 mm(-1), and F(000) = 960. The final agreement factors are R = 0.076 and R-w=0.096 for 1600 observed independent reflections with F greater than or equal to 4.0 sigma (F). The structure revealed that the vanadium atom is bound to two terminal oxygen atoms and one tridentate donor ligand in a distorted square pyramidal arrangement. The sulphur-nitrogen-oxygen donor Schiff-base ligand in the thiol form rather than the thione form is coordinated to the vanadium via the mercapto sulphur, the beta -nitrogen and the hydroxylate oxygen.
A new method for analysing the ingredients of rhynchophylline and isrhynchophylline in Uncaria Rhynchophylla Jacks using hyphenaed high efficiency thin layer chromatographic (TLC) and the surface-enhanced raman spectroscopic (SERS) technics is reported.The results show that the characteristic spectral bands of rhynchophylline can be obtained from the TLC spot with minimum amount of rhynchophylline sample of about 2.5 mm diameter.The difference between the SERS and solid spectra are found.Spectral band at 1 397 cm-1 was obtained wits great enhanced want.Molecule was absorbed in surface silver sol by pair of electrons in -OCH3.Isrhynchophylline sample spectrum band at 1 615 cm-1 obtained the greatest enhance.Isrhynchophylline molecule was absorbed in surface silver sol by pair of electron at N atom in ring indole.An absorption model of rhynchophylline and isrhynchophylline and silver sol is proposed.That effective combination of TLC and SERS can be used to analyse the chemical ingredients with high sensitivity.
A new method for analysing the ingredients of reserpine by thin layer chromatography (TLC) and surface-enhanced Raman spectroscopy (SERS) is reported in this paper. The results show that the characteristic spectral bands of reserpine satuated at the thin layer with the amount of sample about 2 microg were obtained. The difference between SERS and solid spectra was found. An absorption model of reserpine and silver sol was proposed. This method can be used to analyse the chemical ingredients with high sensitivity.