New solid complex of the antimony trichloride and dioxane was obtained th rough a reaction of the dioxane and the absolute methanol solution of the antimony trichloride.The formula of the complex is[SbCl3·｛(CH2)...New solid complex of the antimony trichloride and dioxane was obtained th rough a reaction of the dioxane and the absolute methanol solution of the antimony trichloride.The formula of the complex is[SbCl3·｛(CH2)4O2｝1.5].The crystal structure of the comple x belongs to cubic system,space group I-43d,a=17.1417(5)?,Z =16.The trivalent antimony ion n ot only bonds directly to three chlorine anions,but also is co ordinated by three oxygen atoms of th e dioxane molecules.Two oxygen atoms in a dioxane molecule wi ll coordinate to different antimony ions,respectively.展开更多
目的：建立气相色谱法,同时测定药用辅料中二氯甲烷、三氯甲烷、三氯乙烯、1,4-二氧杂环己烷4种挥发性有机杂质。方法：使用DB-WAX（30.0 m×250μm×0.25μm）弹性毛细管柱,进样口温度200℃,分流比10∶1,恒流流速1.0 m L·...目的：建立气相色谱法,同时测定药用辅料中二氯甲烷、三氯甲烷、三氯乙烯、1,4-二氧杂环己烷4种挥发性有机杂质。方法：使用DB-WAX（30.0 m×250μm×0.25μm）弹性毛细管柱,进样口温度200℃,分流比10∶1,恒流流速1.0 m L·min-1,检测口温度230℃,柱温为程序升温（起始温度35℃,保持5 min,8℃·min-1升至70℃,以50℃·min-1升至180℃）,顶空平衡温度140℃,时间30 min。结果：回收率：二氯甲烷100.3%~100.6%,三氯甲烷101.3%~101.8%,三氯乙烯100.9%~101.4%,1,4-二氧杂环己烷99.6%~100.1%;精密度的RSD：二氯甲烷1.65%,三氯甲烷2.25%,三氯乙烯2.00%,1,4-二氧杂环己烷1.55%。3种辅料中有机挥发性杂质检测结果：交联羧甲基纤维素钠中三氯甲烷质量分数为0.67~1.88μg·g-1,二氯甲烷、三氯乙烯及1,4-二氧杂环己烷未检出;微粉硅胶中二氯甲烷质量分数为1.12~3.25μg·g-1、三氯甲烷、三氯乙烯及1,4-二氧杂环己烷未检出;微晶纤维素中二氯甲烷质量分数为0.91~1.39μg·g-1,三氯甲烷质量分数为1.03~2.36μg·g-1,三氯乙烯质量分数为0.09~0.28μg·g-1,1,4-二氧杂环己烷未检出。结论：本法经方法学验证,适用于交联羧甲基纤维素钠、微粉硅胶及微晶纤维素中有机挥发性杂质的检测。展开更多
Ring opening of extremely hydrophobic epoxides with water, amines, sodium azide and thiophenol was realized in the mixture solvent of water and 1, 4-dioxane under reflux condition. Hot water was believed to act as a m...Ring opening of extremely hydrophobic epoxides with water, amines, sodium azide and thiophenol was realized in the mixture solvent of water and 1, 4-dioxane under reflux condition. Hot water was believed to act as a mild Bronsted acid catalyst in the epoxide-opening reactions.展开更多
A method for oxidative degradation of 1,4-dioxane （1,4-D） in waste water using a combination of ozone oxidation with UV irradiation （ozone/UV） treatment was investigated. The results showed that 1,4-D was degraded...A method for oxidative degradation of 1,4-dioxane （1,4-D） in waste water using a combination of ozone oxidation with UV irradiation （ozone/UV） treatment was investigated. The results showed that 1,4-D was degraded by ozone/UV treatment up to 90 min. The optimum concentration for the injected ozone gas was about 40 g·m^3 under a constant level of UV irradiation. Furthermore, solid phase extraction and GC-MS analysis showed no specific or reproducible peaks due to by-products of 1,4-D. It was therefore concluded that 1,4-D was completely degraded by ozone/UV treatment. In contrast, the amount of 1,4-D remaining decreased slowly in the presence of HCOf or CI. It was suggested that the degradation of 1,4-D, which results from .OH oxidation, was retarded by the presence of HCO3 or CI, which act as radical scavengers.展开更多
文摘New solid complex of the antimony trichloride and dioxane was obtained th rough a reaction of the dioxane and the absolute methanol solution of the antimony trichloride.The formula of the complex is[SbCl3·｛(CH2)4O2｝1.5].The crystal structure of the comple x belongs to cubic system,space group I-43d,a=17.1417(5)?,Z =16.The trivalent antimony ion n ot only bonds directly to three chlorine anions,but also is co ordinated by three oxygen atoms of th e dioxane molecules.Two oxygen atoms in a dioxane molecule wi ll coordinate to different antimony ions,respectively.
基金financially supported by the National Natural Science Foundation of China (20402007, 20772065)Program for New Century Excellent Talents in University+1 种基金the 111 Project (B06005)the National High-tech Research & Development Program of China (863 Projcect, 2006AA020502)
文摘Ring opening of extremely hydrophobic epoxides with water, amines, sodium azide and thiophenol was realized in the mixture solvent of water and 1, 4-dioxane under reflux condition. Hot water was believed to act as a mild Bronsted acid catalyst in the epoxide-opening reactions.
文摘A method for oxidative degradation of 1,4-dioxane （1,4-D） in waste water using a combination of ozone oxidation with UV irradiation （ozone/UV） treatment was investigated. The results showed that 1,4-D was degraded by ozone/UV treatment up to 90 min. The optimum concentration for the injected ozone gas was about 40 g·m^3 under a constant level of UV irradiation. Furthermore, solid phase extraction and GC-MS analysis showed no specific or reproducible peaks due to by-products of 1,4-D. It was therefore concluded that 1,4-D was completely degraded by ozone/UV treatment. In contrast, the amount of 1,4-D remaining decreased slowly in the presence of HCOf or CI. It was suggested that the degradation of 1,4-D, which results from .OH oxidation, was retarded by the presence of HCO3 or CI, which act as radical scavengers.
