Make 1L of solvent system and put this in an Erlenmeyer flask

and swirl
Fill up the graduated cylinder to about 210-220 ml mark with
silica powder (need about 90-100 grams of silica gel) - we used
about 89
Fill up another smaller Erlenmeyer flask with about 250 mL of the
solvent youre using. Also fill up a squirt bottle up a third of the
way with the solvent from the big flask.
Get a bit of glass wool and use the long glass rod to put the glass
wool in the column. Make sure the column is straight.
Put some of the solvent from the big flask into the column with
the stopcock closed.
Put the silica powder in the flask with the 250 ml of solvent, swirl
it to mix. Make sure there are no clumps - becomes a slurry mix.
Take the slurry mix and now put it in the column quickly - make
sure it is mixed. At the same time, open the stopcock so that the
column can start forming. The excess solvent at the bottom will
drain out into a beaker you place below. At some point, before
putting all the slurry in, use the squirt bottle to rinse off and
remove the glass rod. Also use the squirt bottle to rinse off the
inside of the round part of the column. Leave the stopcock open
until the silica settles into the column. Close the stopcock.
When youre ready to load the sample, first fold a filter paper so
that it has wings put that in the column and let it settle. Then
you want to take one pipette full of the solvent system and mix
your sample in it. Then open the stopcock on the column so that
the solvent above the column starts coming out. When there is
almost no solvent on top of the column, youre going to fill a long
pipette with the sample, and slowly drip it out on to the filter
paper that is sitting on the column. Once you have done this,
rinse out the tube that contained the sample with some of the
solvent system and load that as well with the pipette onto the
column. Then you want to take the rest of of your solvent system
flask and slowly add solvent so that it fills the round part of the
flask. You can then pressurize the column with N2 gas or add a
lot of solvent on top.
To adsorb sample to silica. Transfer sample to roundbottom using an
appropriate solvent using however much necessary. Use only 85-90 g
Silica gel to load the column as described above. Add 1 g of Silica gel/
g of material to roundbottom and put on rotovap to take away solvent.
Its good if silica gel becomes a free flowing powder with the sample
adsorbed to it. Sometimes it becomes sticky or gel like.
First fraction should be the largest and put in an Erlenmeyer flask.