Home›Organic Chemistry›Quick vacuum column chromatography: shortcut way of compound purification (VLC)
Steps
1Prepare and pack silica gel column00:24
2Add sand layer and pre-wet column01:50
3Dissolve and load sample onto column02:40
4Protect column with cotton layer03:35
5Add mobile phase and apply vacuum04:05
6Collect fractions and monitor progress05:20
7Continue collection and verify purity07:50
Organic ChemistryYouTube (Curated Tutorials)
Quick vacuum column chromatography: shortcut way of compound purification (VLC)
Protocol
Difficulty
intermediate
Steps
1
Prepare and pack silica gel column
Attach the flash column to a flask and pour silica gel into the column. Apply vacuum to pack the silica evenly without gaps, ensuring an even, level surface with no parabolic inclination.
▶ 00:24
2
Add sand layer and pre-wet column
Place a layer of sand on top of the packed silica gel and add a small amount of solvent to pre-wet the column before sample loading.
▶ 01:50
3
Dissolve and load sample onto column
Dissolve the crude sample in a vial using hackin and ethyl acetate, then carefully pour the dissolved sample onto the sand layer in the column. Perform a second rinse of the vial with ethyl acetate and add this to the column as well.
▶ 02:40
4
Protect column with cotton layer
Place a layer of cotton on top of the silica and sand layers to protect them from disturbance when adding the mobile phase solvent.
▶ 03:35
5
Add mobile phase and apply vacuum
Pour the solvent mixture (2% ethyl acetate in hexane) into the column as the mobile phase. Connect the vacuum line to the bottom of the flash column and turn on the vacuum pump to drive the solvent through the column.
▶ 04:05
6
Collect fractions and monitor progress
Collect approximately 500 mL fractions in separate round-bottom flasks as the solvent flows through. Perform TLC analysis on each collected fraction to identify which fractions contain the pure compound.
▶ 05:20
7
Continue collection and verify purity
Continue changing flasks and collecting new fractions while running additional solvent through the column. Check TLC results to confirm all compounds have eluted and ensure collection of pure product fractions.
▶ 07:50
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