2,2′-Dichlorohydrazobenzene(DHB) was prepared in two steps. o-Chloronitrobenzene( OCNB) was at first reduced to 2,2′-dichloroazoxybenzene(DOB) in aqueous medium using 2,3-dichloro-1,4-naphthaquinone(OCNQ) as catalys...2,2′-Dichlorohydrazobenzene(DHB) was prepared in two steps. o-Chloronitrobenzene( OCNB) was at first reduced to 2,2′-dichloroazoxybenzene(DOB) in aqueous medium using 2,3-dichloro-1,4-naphthaquinone(OCNQ) as catalyst with yield of 99.4%, mp 53～56 ℃; DOB was then reduced by formaldehyde to give DHB in aqueous alkaline methanol with yield of 76%, 49% higher than reported, mp 82～83.5 ℃. DHB could be rearranged to 3,3′-dichlorobenzidine in strong acidic medium with yield 91.8%, mp 132～ 134 ℃.展开更多
建立了气相色谱/质谱来测定土壤中芳香胺3,3′-二氯联苯胺的方法。该化合物通过超声波辅助萃取,选择正己烷-丙酮混合溶剂（体积比为1∶1）或乙酸乙酯,以及Cleanert S C18-SPE柱进行净化。该方法测定土壤中3,3’-二氯联苯胺的检出限为2.8...建立了气相色谱/质谱来测定土壤中芳香胺3,3′-二氯联苯胺的方法。该化合物通过超声波辅助萃取,选择正己烷-丙酮混合溶剂（体积比为1∶1）或乙酸乙酯,以及Cleanert S C18-SPE柱进行净化。该方法测定土壤中3,3’-二氯联苯胺的检出限为2.8μg·kg^-1（信噪比S/N=3）;3,3′-二氯联苯胺的加标回收率平均值为89.7%（n=5）;重复进样RSD为3.55%（n=5）。该方法的线性范围是120-2 400μg·kg^-1,相关系数0.999 5。该方法也可用于沉积物中3,3′-二氯联苯胺的测定。展开更多
文摘2,2′-Dichlorohydrazobenzene(DHB) was prepared in two steps. o-Chloronitrobenzene( OCNB) was at first reduced to 2,2′-dichloroazoxybenzene(DOB) in aqueous medium using 2,3-dichloro-1,4-naphthaquinone(OCNQ) as catalyst with yield of 99.4%, mp 53～56 ℃; DOB was then reduced by formaldehyde to give DHB in aqueous alkaline methanol with yield of 76%, 49% higher than reported, mp 82～83.5 ℃. DHB could be rearranged to 3,3′-dichlorobenzidine in strong acidic medium with yield 91.8%, mp 132～ 134 ℃.
文摘建立了气相色谱/质谱来测定土壤中芳香胺3,3′-二氯联苯胺的方法。该化合物通过超声波辅助萃取,选择正己烷-丙酮混合溶剂（体积比为1∶1）或乙酸乙酯,以及Cleanert S C18-SPE柱进行净化。该方法测定土壤中3,3’-二氯联苯胺的检出限为2.8μg·kg^-1（信噪比S/N=3）;3,3′-二氯联苯胺的加标回收率平均值为89.7%（n=5）;重复进样RSD为3.55%（n=5）。该方法的线性范围是120-2 400μg·kg^-1,相关系数0.999 5。该方法也可用于沉积物中3,3′-二氯联苯胺的测定。
