The fluorescent reaction of salicylaldehyde salicyloylhydrazone(SASH) with indium(Ⅲ) was studied in detail. Based on this chelation reaction, a sensitive spectrofluorimetric method was developed for the determination...The fluorescent reaction of salicylaldehyde salicyloylhydrazone(SASH) with indium(Ⅲ) was studied in detail. Based on this chelation reaction, a sensitive spectrofluorimetric method was developed for the determination of indium in a water ethanol(volume ratio 3∶7) medium at pH 4 0. Under the condition, the In SASH complex displays an excitation and emission maxima at 396 and 461 nm, respectively. The linear range of the method is from 4 7 to 1000 ng/mL and the detection limit is 0 94 ng/mL. The molar ratio of indium to the reagent is 1∶1. The interferences of other ions were studied. The method was successfully applied to the determination of indium in the chemical reagents of lead, tin, zinc, zinc chloride and geological samples by standard addition method.展开更多
オhe fluorescent reagent, salicylaldehyde-5-bromo-salicyloylhydrazone (SABSH) was synthesized and its ionization constants were determined spectrophotometrically. The fluorescent reaction of this reagent with gallium ...オhe fluorescent reagent, salicylaldehyde-5-bromo-salicyloylhydrazone (SABSH) was synthesized and its ionization constants were determined spectrophotometrically. The fluorescent reaction of this reagent with gallium was studied. Based on this chelation reaction, a highly sensitive spectrofluorometric method was developed for the determination of gallium in a ethanol-water (3+2, V/V) medium at pH 2.3. Under these conditions, the GaⅢSABSH complex has excitation and emission maxima at 390 and 457 nm, respectively. The linear range of the method is from 0.0 to 1×10-4 g/L and the detection limit is 4×10-7 g/L of gallium when a standard additions method is used. The molar ratio of gallium to the reagent is 1∶1. Interferences were evaluated. The method was successfully applied to the determination of gallium in soil samples. Extraction with n-butyl acetate from 6 mol/L hydrochloric acid medium was used to separate gallium from the interfering elements in the soil samples.展开更多
The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342...The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342（16）nm, a = 101.696（2）, β = 103.519（2）, γ = 110.744（2）°, V= 1.2329（3） nm^3, Z = 2, Mr = 635.61, F（000） = 628, Dc= 1.712 g/cm^3 and μ（MoKa） = 4.270 mm^-1. The structure was refined to the final R = 0.0524 and wR = 0.1239 for 2763 observed reflections with I 〉 2σ（ I）. The X-ray crystal structure analysis revealed that the center zinc（Ⅱ） is bonded with two oxygen and one nitrogen atoms from a tridentate ligand 3,5-dibromo-salicylaldehyde salicyloylhydrazone （DBSHSH） and two nitrogen atoms from two solvent pyridine molecules to form a distorted five-coordinate trigonal bipyramid. The intramolecular hydrogen bonds in the crystal structure play an important role in the title complex＇s thermostability.展开更多
The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-me...The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine. Similarly, another new complex, [VO(L)(OCH3)] 2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine. Crystal data for 1: C19H15N3O5BrV, Mr= 496.2, monoclinic, P21/n, a = 7.1885(3), b = 9.2718(3), c = 28.803(1) A, β = 96.185(1)°, Z = 4 and V = 1908.6(1) A3; for 2: C15H12N2O5BrV, Mr= 431.1, monoclinic, P2,/n, a = 12.202(2), b = 8.045(2), c = 16.604(3) A, β = 101.29(3)°, Z = 4 and V = 1598.4(2) A3. The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid. Three of the four based donor atoms are from the tridentate 'ONO' donor ligand while the fourth is one terminal oxygen atom with the V(1) - O(3) distance 1.646(4) A for 1 and one -OCH3 group with the V(1)-O(3) distance 1.753(3) A for 2. The V(1)-O(4) terminals occupy the axial sites in both cases. The complexes are also characterized by IR and 1H NMR spectroscopies.展开更多
文摘The fluorescent reaction of salicylaldehyde salicyloylhydrazone(SASH) with indium(Ⅲ) was studied in detail. Based on this chelation reaction, a sensitive spectrofluorimetric method was developed for the determination of indium in a water ethanol(volume ratio 3∶7) medium at pH 4 0. Under the condition, the In SASH complex displays an excitation and emission maxima at 396 and 461 nm, respectively. The linear range of the method is from 4 7 to 1000 ng/mL and the detection limit is 0 94 ng/mL. The molar ratio of indium to the reagent is 1∶1. The interferences of other ions were studied. The method was successfully applied to the determination of indium in the chemical reagents of lead, tin, zinc, zinc chloride and geological samples by standard addition method.
文摘オhe fluorescent reagent, salicylaldehyde-5-bromo-salicyloylhydrazone (SABSH) was synthesized and its ionization constants were determined spectrophotometrically. The fluorescent reaction of this reagent with gallium was studied. Based on this chelation reaction, a highly sensitive spectrofluorometric method was developed for the determination of gallium in a ethanol-water (3+2, V/V) medium at pH 2.3. Under these conditions, the GaⅢSABSH complex has excitation and emission maxima at 390 and 457 nm, respectively. The linear range of the method is from 0.0 to 1×10-4 g/L and the detection limit is 4×10-7 g/L of gallium when a standard additions method is used. The molar ratio of gallium to the reagent is 1∶1. Interferences were evaluated. The method was successfully applied to the determination of gallium in soil samples. Extraction with n-butyl acetate from 6 mol/L hydrochloric acid medium was used to separate gallium from the interfering elements in the soil samples.
基金The project was supported by the Natural Science Education of Hubei Province (No. 2001A27006)
文摘The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342（16）nm, a = 101.696（2）, β = 103.519（2）, γ = 110.744（2）°, V= 1.2329（3） nm^3, Z = 2, Mr = 635.61, F（000） = 628, Dc= 1.712 g/cm^3 and μ（MoKa） = 4.270 mm^-1. The structure was refined to the final R = 0.0524 and wR = 0.1239 for 2763 observed reflections with I 〉 2σ（ I）. The X-ray crystal structure analysis revealed that the center zinc（Ⅱ） is bonded with two oxygen and one nitrogen atoms from a tridentate ligand 3,5-dibromo-salicylaldehyde salicyloylhydrazone （DBSHSH） and two nitrogen atoms from two solvent pyridine molecules to form a distorted five-coordinate trigonal bipyramid. The intramolecular hydrogen bonds in the crystal structure play an important role in the title complex＇s thermostability.
基金The work was supported by the Chinese Academy of Sciences, the National Natural Science Foundation of China(20073048)the NSF of Fujian province for financial support
文摘The new oxovanadium (V) complex, [PyH][VO2(L)] 1 (salicyladehyde 5-bromo salicyloylhydrazone is abbreviated as H2L; Hpy is protonated pyridine) was obtained from a refluxed solution of VOSO4 and H2L in acetonitrile-methanol-pyridine. Similarly, another new complex, [VO(L)(OCH3)] 2 was synthesized by refluxing VOSO4 and H2L in methanol-pyridine. Crystal data for 1: C19H15N3O5BrV, Mr= 496.2, monoclinic, P21/n, a = 7.1885(3), b = 9.2718(3), c = 28.803(1) A, β = 96.185(1)°, Z = 4 and V = 1908.6(1) A3; for 2: C15H12N2O5BrV, Mr= 431.1, monoclinic, P2,/n, a = 12.202(2), b = 8.045(2), c = 16.604(3) A, β = 101.29(3)°, Z = 4 and V = 1598.4(2) A3. The structures of 1 and 2 have been determined by X-ray analyses and reveal that the coordination environments of V atoms in both complexes are of square-based pyramid. Three of the four based donor atoms are from the tridentate 'ONO' donor ligand while the fourth is one terminal oxygen atom with the V(1) - O(3) distance 1.646(4) A for 1 and one -OCH3 group with the V(1)-O(3) distance 1.753(3) A for 2. The V(1)-O(4) terminals occupy the axial sites in both cases. The complexes are also characterized by IR and 1H NMR spectroscopies.
