Objective: to isolate vanillin from a black commercial vanilla extract using a very simple and homemade column chromatography device.

Procedure: a 10ml syringe was filled to the 10ml mark with cotton pressed as hard as possible (1). It was placed hanging from the mouth of a bottle and fully soaked with ethanol 96% (2). 0.5ml of black commercial vanilla extract (3) were carefully placed on the top of the syringe. The vanilla was allowed to settle and a thin layer of starch (could also be sand) was placed on top. At first, pure ethanol was recovered from the bottom while more ethanol was continuously added on top. Before the brown layer reached the bottom (~20min), a first clear fraction was obtained. A second light brown fraction was obtained and stored; the rest was discarded (4). The first fraction was allowed to almost completely evaporate, yielding a clean white solution with a very strong vanilla odor (5).

Conclusion: it is not known if the obtained solution is pure vanillin (most probably it's not), but good results were obtained using very simple and cheap stuff.

(1)


(2): the column is already pretty washed here.


(3)


(4)


(5)

That's interesting, what other stuff can be separated using this? is it possible to separate excess salt from harmala-hcl using this?

That's really nice but wet columns are quite cheap so why bother (aside from the sheer exhilaration of building it yourself) ?

yes, using a basic aqueous mobile phase, like dilute ammonia. salts are small, so they'll elute first. then you elute with a nonpolar like dcm to collect your alks

and obviously, you don't want to use nonpolar solvents in a makeshift plastic column.