点板(TLC)极性最大展开剂怎么配

Organic Route 有机合成路线 2023-03-06 08:36

合成化学离不开溶剂,比如其可以作为反应介质,过柱子纯化可以作为洗脱剂,萃取也需要等等。TLC点板需要我们配置展开剂,那么这就需要我们了解各种溶剂的性质和极性大小,那么TLC极性最大展开剂怎么配?

 

有机溶剂极性表

 

常用混合溶剂极性顺序

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常用混合溶剂

1) 乙酸乙酯/己烷:常用浓度0~30%。但有时较难在旋转蒸发仪上完全除去溶剂。 

2乙醚/戊烷体系:浓度为0~40%的比较常用。在旋转蒸发器上非常容易除去。 

乙醇/己烷或戊烷:对强极性化合物5~30%比较合适。 

二氯甲烷/己烷或戊烷:5~30%,当其他混合溶剂失败时可以考虑使用。 

3) 将1~2mL选定的溶剂体系倒入展开池中,在展开池中放置一大块滤纸。 

4) 将化合物在标记过的基线处进行点样。我们用的点样器是买来的,此外点样器也可从加热过的Pasteur吸管上拔下(你可以参照UROP)。在跟踪反应进行时,一定要点上起始反应物、反应混合物以及两者的混合物。 

5) 展开:让溶剂向上展开约90%的薄板长度。 

6) 从展开池中取出薄板并且马上用铅笔标注出溶剂到达的前沿位置。根据这个算Rf的数值。 

7) 让薄板上的溶剂挥发掉。 

8) 用非破坏性技术观察薄板。最好的非破坏性方法就是用紫外灯进行观察。将薄板放在紫外灯下,用铅笔标出所有有紫外活性的点。尽管在5.301中不用这种方法,但我们将采用另一常用的无损方法--用碘染色法。(你可以参看UROP)。 

9) 用破坏性方式观测薄板。当化合物没有紫外活性的时候,只能采用这种方法。在5.301中,提供了很多非常有用的染色剂。使用染色剂时,将干燥的薄板用镊子夹起并放入染色剂中,确保从基线到溶剂前沿都被浸没。用纸巾擦干薄板的背面。将薄板放在加热板上观察斑点的变化。在斑点变得可见而且背景颜色未能遮盖住斑点之前,将薄板从加热板上取下。 

10) 根据初始薄层色谱结果修改溶剂体系的选择。如果想让Rf变得更大一些,可使溶剂体系极性更强些;如果想让Rf变小,就应该使溶剂体系的极性减小些。如果在薄板上点样变成了条纹状而不是一个圆圈状,那么你的样品浓度可能太高了。稀释样品后再进行一次薄板层析,如果还是不能奏效,就应该考虑换一种溶剂体系。 

来源:网络,仅供交流学习!原文链接:http://muchong.com/t-3430257-1

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