十溴联苯醚萃取条件优化研究

Optimization of decabromodiphenyl ether extraction conditions

针对十溴联苯醚(BDE-209)难溶性和萃取方法的复杂性,通过从萃取剂和萃取条件上对BDE-209进行萃取优化。结果表明:(1)上清-沉淀复合法的萃取效率仅为21.8%。(2)烘干温度对样品的萃取效率影响不显著,在80、 100和120℃条件下的萃取效率均达到95%以上,但高温条件有可能使BDE-209发生降解。(3)不同萃取剂和分步萃取对样品萃取效率影响显著,2次萃取比一次性萃取的萃取效率提高了13.6%~29.6%,正己烷萃取效率(100%)>乙酸乙酯萃取效率(84.87%)>异辛烷萃取效率(23.33%)。(4)采用正己烷少量多次萃取,可短时间内最大程度回收水相样品中的BDE-209(97.82%)。少量多次萃取法萃取效率高,操作简便,节省时间,适于大部分水相样品快速定量分析。

In view of the poor solubility of decabromodiphenyl ether(BDE-209) and the complexity of the extraction method, the extraction of BDE-209 was optimized from aspects of extractant and extraction methods.The results showed that,(1) the extraction efficiency of supernatant/precipitation composite method was only21.8%.(2)Backing temperature has no obvious impact on extraction effect, the extraction efficiency all reached above 95% at 80, 100 and 120 ℃, however, BDE-209 could be degraded under high temperature.(3)Different extractants and steps had significant affect on extraction efficiency of samples, and the efficiency of two-step extraction was 13.6%-29.6% higher than that of the one-time extraction, the extraction efficiencies of n-hexane,ethyl acetate and isooctane were 100%, 84.87% and 23.33% respectively.(4) BDE-209(97.82%) in aqueous samples could be recovered in a short time by n-hexane using small amount of multiple extraction method. Small amount of multiple extraction method has advantages of high extraction efficiency, simple operation and time saving, which is suitable for rapid quantitative analysis of most water phase samples.