利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0....利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0.5 mL氨基磺酸铵除去多余的NaNO2,加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色,快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15 mg/kg,上千个实际样品测试无假阴性,假阳性概率为28%。本方法无需大型色谱仪器设备,与仪器测定方法相比,前处理时间缩短了约60%,节约了约90%的试剂费用。展开更多
根据芳香胺重氮化-偶合显色反应原理,建立了纺织品中4-氨基偶氮苯的快速定性检测方法.纺织品初步还原后,首先用10 m L叔丁基甲醚萃取,再用5 m L HCl进行反萃取,依次加入亚硝酸钠、氨基磺酸铵、邻甲氧基苯酚进行显色.根据显色液是否显红...根据芳香胺重氮化-偶合显色反应原理,建立了纺织品中4-氨基偶氮苯的快速定性检测方法.纺织品初步还原后,首先用10 m L叔丁基甲醚萃取,再用5 m L HCl进行反萃取,依次加入亚硝酸钠、氨基磺酸铵、邻甲氧基苯酚进行显色.根据显色液是否显红色,快速确定纺织品中是否含有4-氨基偶氮苯.与仪器测定方法相比,前处理步骤简化,试剂成本降低;利用显色法测定4-氨基偶氮苯,解决了传统测定方法对大型色谱仪器的依赖.展开更多
使用酚二磺酸法、还原蒸馏法、镀铜镉还原-重氮化偶合比色法和改进紫外分光光度法(校正因数法)测定了中国9种不同类型土壤的硝态氮含量,分析了改进紫外分光光度法与其余三种测定方法的差异及其适用性。统计分析表明对于有机质含量低于50...使用酚二磺酸法、还原蒸馏法、镀铜镉还原-重氮化偶合比色法和改进紫外分光光度法(校正因数法)测定了中国9种不同类型土壤的硝态氮含量,分析了改进紫外分光光度法与其余三种测定方法的差异及其适用性。统计分析表明对于有机质含量低于50 g kg-1的矿质土壤,可以使用2.2作为校正因数,四种分析方法的测定值具有极显著的相关性,尤其是紫外分光光度法与酚二磺酸法的测定结果最为接近,没有极显著差异;对于有机质含量接近和高于50 g kg-1的土壤,校正因数还需要修改。紫外分光光度法具有操作简单、测定速度快等优点,适用于批量快速测定。展开更多
Diazo compounds are generally used as carbene precursors. Traditionally, dirhodium, copper and iron catalysts were used to decompose diazo compounds to form the key metal carbene intermediates. Recently, the gold cata...Diazo compounds are generally used as carbene precursors. Traditionally, dirhodium, copper and iron catalysts were used to decompose diazo compounds to form the key metal carbene intermediates. Recently, the gold catalysts have been developed as a unique type of metal catalyst to decompose diazo compounds. The derived gold carbene showed much different characters comparing with other transition metal carbenes. They could go through a series of cycloaddition, insertion and coupling reactions. Here, the recent progress of the gold carbene chemistry from diazo compounds was reviewed, including the scope of reactions,mechanism and synthetic applications.展开更多
文摘利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0.5 mL氨基磺酸铵除去多余的NaNO2,加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色,快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15 mg/kg,上千个实际样品测试无假阴性,假阳性概率为28%。本方法无需大型色谱仪器设备,与仪器测定方法相比,前处理时间缩短了约60%,节约了约90%的试剂费用。
文摘根据芳香胺重氮化-偶合显色反应原理,建立了纺织品中4-氨基偶氮苯的快速定性检测方法.纺织品初步还原后,首先用10 m L叔丁基甲醚萃取,再用5 m L HCl进行反萃取,依次加入亚硝酸钠、氨基磺酸铵、邻甲氧基苯酚进行显色.根据显色液是否显红色,快速确定纺织品中是否含有4-氨基偶氮苯.与仪器测定方法相比,前处理步骤简化,试剂成本降低;利用显色法测定4-氨基偶氮苯,解决了传统测定方法对大型色谱仪器的依赖.
文摘使用酚二磺酸法、还原蒸馏法、镀铜镉还原-重氮化偶合比色法和改进紫外分光光度法(校正因数法)测定了中国9种不同类型土壤的硝态氮含量,分析了改进紫外分光光度法与其余三种测定方法的差异及其适用性。统计分析表明对于有机质含量低于50 g kg-1的矿质土壤,可以使用2.2作为校正因数,四种分析方法的测定值具有极显著的相关性,尤其是紫外分光光度法与酚二磺酸法的测定结果最为接近,没有极显著差异;对于有机质含量接近和高于50 g kg-1的土壤,校正因数还需要修改。紫外分光光度法具有操作简单、测定速度快等优点,适用于批量快速测定。
基金supported by the National Natural Science Foundation of China(21372144)China Postdoctoral Science Foundation,the Fundamental Research Funds of Shandong University(2014JC008)the Subject Construction Funds of Shandong University(104.205.2.5)
文摘Diazo compounds are generally used as carbene precursors. Traditionally, dirhodium, copper and iron catalysts were used to decompose diazo compounds to form the key metal carbene intermediates. Recently, the gold catalysts have been developed as a unique type of metal catalyst to decompose diazo compounds. The derived gold carbene showed much different characters comparing with other transition metal carbenes. They could go through a series of cycloaddition, insertion and coupling reactions. Here, the recent progress of the gold carbene chemistry from diazo compounds was reviewed, including the scope of reactions,mechanism and synthetic applications.
