You should just be making a slurry and pouring it down the side of the column, settling, and draining.
2 Likes
That’s for the wet loading of solution, correct?
For packing the column.
You take your media, add your mobile phase to 1.5x volume- stir it up real good (stirring in an ultrasonic bath is best because any trapped air bubbles are purged out)
And then pour it into the column, down the side gently, so that you don’t trap air bubbles.
Then ensure the column is level and let the dust settle.
(let it sit for at least one hour, preferably overnight)
When it’s settled, take a piece of fast filter paper and cut it so it fits the column perfectly, ever so slightly smaller than the ID of the column- fold it in half and wet it, then gently, gently lower it down the column, placing it with the end of a skewer or lab spatula and careful not to disturb the bed
You can further protect the integrity of the bed by adding a thin layer of clean sand, but the filter paper works fine for me- just be really light and gentle and let it settle.
The less you fuck with it, the cleaner it’ll be.
2 Likes
Also, you don’t need sand on the base of your column if you have a frit like that- just protect the frit with a filter paper and load media on top.
I would use a separate column for each type of media
2 Likes
I had not seen this described anywhere! Thank you so much @Rowan, that’s hugely helpful.
How long do you sonicate for, or are you more looking the air bubbles to die off?
Would you mind elaborating on that a bit? Are you suggesting for example, say 2 columns one with silica and the other with b80 and running solution through them separately? If so, may I ask why? Is it easier to re-use media that way?
You can clean silica really easily, but b80 works more as an adsorbant and is cheaper-
I just like to keep things separate in case there is an issue with one of the products I can narrow it down more easily and the lifetimes of each media is gonna be very different so it just keeps things uncomplicated
1 Like
Phase contactor.
A whole bunch of filter plates with steel wool stuffed right.
Pour water in top, it travels throughout the maze of wool and makes for a lot of surface area contact without need for agitation.
You’ll never make an emulsion again.
2 Likes
Seriously cool setup! I’ll see what I can MacGyver 
I kind of like the idea of having separate columns setup perpetually (assuming this kind of clean up is a typical occurrence), and I especially like the possibility of reusing the media longer! (Plus I like having backups). So essentially, re-use the expensive silica column and dump the cheap b80 (or t5 or whatever) media?
1 Like
Or LLE device called “Perforator”, not unlike a Soxhlet. Lighter solvent drips through a tube that reaches to the bottom of the heavier phase, exits tube and travels up a spiral path, collects above the heavier phase, then overflows and returns to boiling flask, repeat.
Once you start digging into the elegance of the various LLE apparatus, the sep funnel is practically barbaric.
3 Likes
If I wanted to rig something like this up would something like this work as a phase contractor?
Top down:
High flow peristaltic pump
KF-25 3 way tee
- side port: KF-25 10mm
- top: open to vent gases
12” long extension tube stuffed with stainless steel wool
Sight glass piece
KF-25 3 way Tee
- side port: KF-25 10mm adapter (to circulate back to the top of the column)
- bottom port: KF-25 ball valve with KF-25 10mm adapter (for emptying the column)
Hook the tubing up to the ports, secured with worm gear clamps. Run the peristaltic pump drawing from the bottom and running it through the top.
1 Like
Sweet, Makes sense now i have to make one and try it out. Might be able to use a heat coil on a ss tube to get the circulation going using the rising heat. Could even run a rxn in it with a reflux on top. Kinda like one of those bubbler compost tea barrels.
2 Likes