The electrochemiluminescence (ECL) of a new reagent 6- (2-hydroxy- 4 diethy laminophenylazo)-2,3-dihydro-1 ,4-phthalazine-1,4-dione (HDEA) in a basic aqueous so lution was studied by using the apparatus designed by ou...The electrochemiluminescence (ECL) of a new reagent 6- (2-hydroxy- 4 diethy laminophenylazo)-2,3-dihydro-1 ,4-phthalazine-1,4-dione (HDEA) in a basic aqueous so lution was studied by using the apparatus designed by ourselves. Trace amounts of silver ( Ⅰ ) shows a significant effect on the efficiency of light emission of HDEA during a positive trigonometrical wave pulse was exerted on the solution. The linear relationship between the light intensity and the concentration of silver( Ⅰ ) occurs in the range of 5. 0×10-8 to 3. 0×10-8 mol/L Ag(Ⅰ ) in a medium of KOH-KCl-HDEA (pH= 12. 8). The detection limit of the method is 2. 0×10-8 mol/LAg( Ⅰ ), and the r. s. d. for 1.0×10-7 mo)/L Ag ( Ⅰ ) is 5%. Of 21 metal ions concerned, only nickel( Ⅱ ), cerium( Ⅳ ) and cobalt( Ⅱ ) interfere the silver detection seriously; Ⅰ and Br also have some interference.展开更多
Some transition metal chelates of two ligands L1 and L2 were prepared and characterized by elemental analysis. The IR and 1H NMR spectra of several chelates of two ligands L1 and L2 showed the involvement of the azo g...Some transition metal chelates of two ligands L1 and L2 were prepared and characterized by elemental analysis. The IR and 1H NMR spectra of several chelates of two ligands L1 and L2 showed the involvement of the azo group in chelation with the transition metaI ions, in most of the studied chelates, and that the two ligands L1 and L2 showed the involvement of the azo group in chelation with the transition metal ions, in most of the studied chelates, and that the two ligands L1 and L2 were coordinated either in the enol or the keto form. IR spetra also showed that Fe(III)-, Ni(II)-, Mn(II)-, VO(II)-L1 and Cu(II)-L2 chelates behaved in a bidentate manner, in contrast with the two (1:1) M:L cobalt chelates with the two ligands are tridentate.TG analysis indicated the presence of three to twelve water molecules of hydration eliminated on heating up to 150℃ and one or two coordinated water molecules removed at 150~180℃.The octahedral structure is proposed fOr all the chelates, except Cu(II)-L2 and Ni(II)-L1 chelates which have square planar geometry, based on their electronic spectra展开更多
文摘The electrochemiluminescence (ECL) of a new reagent 6- (2-hydroxy- 4 diethy laminophenylazo)-2,3-dihydro-1 ,4-phthalazine-1,4-dione (HDEA) in a basic aqueous so lution was studied by using the apparatus designed by ourselves. Trace amounts of silver ( Ⅰ ) shows a significant effect on the efficiency of light emission of HDEA during a positive trigonometrical wave pulse was exerted on the solution. The linear relationship between the light intensity and the concentration of silver( Ⅰ ) occurs in the range of 5. 0×10-8 to 3. 0×10-8 mol/L Ag(Ⅰ ) in a medium of KOH-KCl-HDEA (pH= 12. 8). The detection limit of the method is 2. 0×10-8 mol/LAg( Ⅰ ), and the r. s. d. for 1.0×10-7 mo)/L Ag ( Ⅰ ) is 5%. Of 21 metal ions concerned, only nickel( Ⅱ ), cerium( Ⅳ ) and cobalt( Ⅱ ) interfere the silver detection seriously; Ⅰ and Br also have some interference.
文摘Some transition metal chelates of two ligands L1 and L2 were prepared and characterized by elemental analysis. The IR and 1H NMR spectra of several chelates of two ligands L1 and L2 showed the involvement of the azo group in chelation with the transition metaI ions, in most of the studied chelates, and that the two ligands L1 and L2 showed the involvement of the azo group in chelation with the transition metal ions, in most of the studied chelates, and that the two ligands L1 and L2 were coordinated either in the enol or the keto form. IR spetra also showed that Fe(III)-, Ni(II)-, Mn(II)-, VO(II)-L1 and Cu(II)-L2 chelates behaved in a bidentate manner, in contrast with the two (1:1) M:L cobalt chelates with the two ligands are tridentate.TG analysis indicated the presence of three to twelve water molecules of hydration eliminated on heating up to 150℃ and one or two coordinated water molecules removed at 150~180℃.The octahedral structure is proposed fOr all the chelates, except Cu(II)-L2 and Ni(II)-L1 chelates which have square planar geometry, based on their electronic spectra