Ever heard about Colum Chromatography? If not, than have a quick look at the general principle, which was briefly presented by @mcw. It is also closely related to Thin Layer Chromatography or TLC, another topic he discussed earlier.
Building upon this I would like to share some funny 'purification setup', which I was needed to use in the lab lately:
The smallest and cutest Chromatography Column
Tiny Chromatography Column: Pasteur Pipette, Cotton & Silica Gel
I was challenged to selectively convert a certain sec. alcohol into an ketone functionality. For this I used the so-called TPAP oxidation, which works with Tetrapropylammonium perruthenate ('TPAP') as an oxidation catalyst and N-Methylmorpholine N-oxide ('NMO') as the actual oxidant:
Reaction drawn with ChemSketch freeware
After performing the oxidation step testwise on a microgram scale, I had to analyze the reaction mixture, what required the separation of the catalyst. Since the catalyst is an ionic species, it has enormously strong interaction with the silica gel used as the column material.
This means that the black catalyst did not pass through the tiny column, but got stuck as a black ‘start spot’ right at the beginning of it, rendering this separation more filtration like rather than classical chromatography. Only the other chemical species of the reaction mixture were quickly flushed through the column. So I was able to prepare my mini reaction mixture for analysis with not even five minutes of work.
I hope you enjoyed today's 'tiny’ lab-experience sharing.
Best,
mountain.phil28
That's tiny! What's it look like after the process is done?
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The very top layer of the silica gel was blackened, since the black ruthenium cat adsorbed there and the before black reaction mixture was colorless and translucent afterwards. - Sry, did not take a second photograph then.
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NICEEEEEE!!!!
TPAP/NMO!!!! RICHHHHHHHHHHHH XDD
I was doing the swern oxidation cuz we r run out of TPAP at that time T.T
Pipette column is a essential technique for a synthetic chemist XDDDDDDDDD
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Haha ja i also used the last few grains of TPAP. :)
I call this VLHTPCC: Very Limited High Throughput Column Chromatography ! Haha!
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Wa ka ka !!!!
This is really convenient to do a test reaction. Quick "filtration" then is ready for NMR or HPLC-MS analysis
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...don't forget my favorite one: GC-MS :)
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Haha I haven't use GC in my research life yet. (I am really bad with analytical chemistry..... what makes it as your favorate ? or you work on very volatile molecules?)
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I work with rather volatile compounds, the interface between GC and MS is more reliable and robust and you also do not have to refill the eluent every (few) day(s) but just use a big bottle for your carrier gas and then you are happy for a month. :D
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Until the helium tank develops a leak you can't track down. Guess what my current lab problem is. ;)
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Ouch, that's a pity. :D
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