Four solid complexes of alkaline earth picrates with N,N,N′,N′-tetraphenyl-3,6,9-tri- oxaundecanediamide (TTD), M (Pic)2TTD (1, M = Mg; 2, M = Ca; 3, M = Sr; 4, M = Ba), have been prepared and characterized by eleme...Four solid complexes of alkaline earth picrates with N,N,N′,N′-tetraphenyl-3,6,9-tri- oxaundecanediamide (TTD), M (Pic)2TTD (1, M = Mg; 2, M = Ca; 3, M = Sr; 4, M = Ba), have been prepared and characterized by elemental analysis, conductivity measurement, IR spectra, 1H NMR spectra and TG-DTA techniques. Crystal structure of complex 3 shows that the Sr(Ⅱ) ion is 9-coordinated by five oxygen atoms from TTD and four oxygen atoms from two bidentate picrates, and the coordination polyhedron is distorted tricapped trigonal prism. TTD as a pentadentate ligand forms a right-handed helical coordination structure. The chelating helical chain has a rela-tive fixed radius and then shows a high coordination selectivity to metal ion. The high selectivity of TTD to alkaline earth ions is explained elementarily from the special coordination structures.展开更多
A novel solid phase microextraction(SPME) fiber coated with open chain crown ether( α,ω diallyltriethlene glycol, DATEG)/hydroxy terminated silicone oil(OH TSO) was prepared by sol gel approach and cross linking ste...A novel solid phase microextraction(SPME) fiber coated with open chain crown ether( α,ω diallyltriethlene glycol, DATEG)/hydroxy terminated silicone oil(OH TSO) was prepared by sol gel approach and cross linking step. The adsorption and desorption properties of the new SPME fiber to polar compounds such as aromatic amines, non polar compounds such as benzene homologue and high boiling compound such as phthalate esters were investigated by SPME coupled with GC FID, and the results were compared with those of commercially available fibers. The new coating provided a better extraction efficiency and possessed a significantly stable performance at a high temperature(>300 ℃) in solvents, as well as long life span(>200 times). Under the experimental conditions used, the detection limits were 0 1-1 5 μg/L for aromatic amines and 0 03-0 3 μg/L for benzene homologue, and the precisions were below 8%( n =5).展开更多
基金This work was supported by the National Natural Science Foundation of China(Grant No.20071015)Key Project of Science and Technology of the Ministry of Education of China(Grant No.01170)Foundation for University Key Teacher by the Ministry of Education of China.
文摘Four solid complexes of alkaline earth picrates with N,N,N′,N′-tetraphenyl-3,6,9-tri- oxaundecanediamide (TTD), M (Pic)2TTD (1, M = Mg; 2, M = Ca; 3, M = Sr; 4, M = Ba), have been prepared and characterized by elemental analysis, conductivity measurement, IR spectra, 1H NMR spectra and TG-DTA techniques. Crystal structure of complex 3 shows that the Sr(Ⅱ) ion is 9-coordinated by five oxygen atoms from TTD and four oxygen atoms from two bidentate picrates, and the coordination polyhedron is distorted tricapped trigonal prism. TTD as a pentadentate ligand forms a right-handed helical coordination structure. The chelating helical chain has a rela-tive fixed radius and then shows a high coordination selectivity to metal ion. The high selectivity of TTD to alkaline earth ions is explained elementarily from the special coordination structures.
文摘A novel solid phase microextraction(SPME) fiber coated with open chain crown ether( α,ω diallyltriethlene glycol, DATEG)/hydroxy terminated silicone oil(OH TSO) was prepared by sol gel approach and cross linking step. The adsorption and desorption properties of the new SPME fiber to polar compounds such as aromatic amines, non polar compounds such as benzene homologue and high boiling compound such as phthalate esters were investigated by SPME coupled with GC FID, and the results were compared with those of commercially available fibers. The new coating provided a better extraction efficiency and possessed a significantly stable performance at a high temperature(>300 ℃) in solvents, as well as long life span(>200 times). Under the experimental conditions used, the detection limits were 0 1-1 5 μg/L for aromatic amines and 0 03-0 3 μg/L for benzene homologue, and the precisions were below 8%( n =5).
