溶剂选择

2025-03-26 09:10:03
推荐回答(1个)
回答1:

由于每种待测物及环境样品性质不尽相同,这就要对提取溶剂进行优化。根据相似相溶的原理,尽量选择与待测物极性相近的有机溶剂作为提取剂。提取剂必须与样品能很好地分离,且不影响待测物的纯化与测定;提取剂不能与样品发生作用,要求毒性低、价格便宜;此外,还要求提取剂沸点范围在45~80℃之间为好。同时还要考虑溶剂对样品的渗透力,以便将土样中待测物充分提取出来。当单一溶剂不能成为理想的提取剂时,常用两种或两种以上不同极性的溶剂以不同的比例配成混合提取剂。《土壤环境监测技术规范》(HJ/T166—2004)中提到的常用有机溶剂的极性由强到弱的顺序为:水、腈、甲醇、乙酸、乙醇、异丙醇、丙酮、二氧六环、正丁醇、正戊醇、乙酸乙酯、乙醚、硝基甲烷、二氯甲烷、苯、甲苯、二甲苯、四氯化碳、二硫化碳、环己烷、正己烷(石油醚)和正庚烷。

由于溶剂种类很多,如果全面展开,仅溶剂一项就会成本很高、耗时很长。本实验仅选择了文献中几种常用溶剂———甲醇、丙酮、正己烷和二氯甲烷,以超声提取为处理方法分别对土壤样品(均为10g)中16种多环芳烃和8种有机氯农药进行实验。

不同溶剂对土壤样品中16种多环芳烃提取结果见表2.5。

表2.5 多环芳烃提取结果(单位:ng)

图2.8可以更直观地显示测量结果。

图2.8 不同溶剂对PAHs提取结果

结果表明:不同溶剂对多环芳烃的提取效果差异较大。单一溶剂中,甲醇效果最差,正己烷和丙酮效果次之,二氯甲烷提取效果最好,特别是对四环及其以上的多环芳烃提取优势明显,例如苯并[a]芘、茚[1,2,3-cd]芘、苯并[a,h]蒽和苯并[g,h,i]苝等;单一溶剂的提取效果并非与其极性强度成正比。由此可以得出:极性过强或过弱的溶剂不适宜对多环芳烃的提取,只有极性在一定范围内的有机溶剂才有助于土壤中多环芳烃的提取。

所选择的溶剂中,整体效果上看,正己烷∶二氯甲烷=1∶1提取效果最好。这是由于不同溶剂极性不同、渗透力不同,相互间产生促萃效应,弥补了彼此的不足,进而对土壤样品中多环芳烃产生了较好的萃取能力。不同溶剂对土壤样品中的有机氯农药提取结果见表2.6。

表2.6 有机氯农药提取结果(单位:ng)

图2.9可以更直观显示测量结果。

图2.9 不同溶剂对有机氯农药提取结果

结果表明:不同溶剂对有机氯农药的提取效果明显不同。单一溶剂中,甲醇效果最差,正己烷效果次之,丙酮和二氯甲烷提取效果最好,对DDT提取效果看丙酮稍显优势。实验结果并非完全与溶剂极性强度成正比。由此可以得出:极性过强或过弱的溶剂亦不适宜对有机氯农药的提取,只有极性在一定范围内的有机溶剂才有助于土壤中有机氯农药的提取。

所选择的溶剂中,整体效果上看,正己烷∶二氯甲烷=1∶1提取效果最好,对八种有机氯农药均表现出较好的提取效果,而丙酮∶二氯甲烷=1∶1的提取效果稍差于前者,正己烷∶丙酮=1∶1的混合溶剂的提取效果与前两者相比较,则显出对DDT的提取效果较差。整体上看混合溶剂正己烷∶二氯甲烷=1∶1对土壤中的有机氯农药提取效果均优于单一溶剂。这是由于不同溶剂极性不同、渗透力不同,相互间产生促萃效应,弥补了彼此的不足,进而对土壤样品中有机氯农药产生了较好的萃取能力。

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