Column chromatography for honey oil

[coledog855]

Sorry, I was pretty high last time I posted, so my post sounded pretty stupid

Looking at what would have to go into this, you might not yield that much thc from the amount of bud you will be using. I think to make this worth it, you'd have to use some very potent bud, and then the yield from each level of filtration will be less than the original amount, meaning you might lose 10 or more dollars out of every 50 you invest in bud. If you are willing to spend some money to get high like very few have ever done in this country, then I say you should go for it.

Just think about this. If extracting pure THC was easy or even remotely cost efficient, then we'd see a lot less green on the streets b/c moving clear THC would be much easier to make money off of.

[vostro]

I agree, and I think that reasoning is sound.

I think a further reason that you don't see clear/pure THC oil, is that pure THC will yield a high that is not necessarily as enjoyable as the high you get with the intoxication of the other cannabinoids - there are other psychoactive cannabinoids.

People who take Marinol pills, which are purified THC and sesame oil, describe the experience as taking a long time to set on (maybe the result of gastric administration ) and the high being so intense it was scary and unenjoyable. If that weren't the case, the continued press for the legalization, besides access and cost issues, wouldn't continue. My dad had cancer and was prescribed Marinol for nausea, but bought some bud and smoked it instead because he said he didn't like the effect of the pure-Marinol THC.

Also I think maybe it's a psychological thing. Kind of like at a secret santa people like to get the biggest box. When you buy bud and get a big hefty smelly bag of green I think there's some kind of gratification in that, which doesn't come with buying a little vile of clear liquid. There are other benefits also- buying something straight off of a plant it's easy to tell that it's not laced with something, you can see what you're getting. I guess with other, hard drugs, you just hope what you bought doesn't kill you. You'd be creating that situation with marijuana if they sold it in clear oil form.

That said, I think with just a hot plate, beaker, Büchner funnel flask, charcoal, chloroform, and Graham condenser (for refluxing), you could make some extremely clean, potent honey oil (especially if you started with a strain like Cinderella 99) and those things combined don't cost that much, maybe $150-200 used. The Soxhlet and rotovap would be nice but not really necessary, and too expensive to buy per the advantage if you don't already have access to that stuff. The column chromatography is chiefly for separating the THC from the other cannabinoids- so if you're looking for a more potent version of the high you normally get from smoking you wouldn't want that anyway.

[gordonliu]

Yes I realize that this is a very old thread, but I am sure there are new generations of little kids getting all excited about cannabis, googling the hell out of it, and falling asleep to dreams of the most ultra-potent honey oil known to man.


Let me first give you the, unfortunately negative, "death of your dreams" comment that all forum posters hear:

its never gonna happen, its a waste of time and money, and its too difficult if you are asking questions on a forum.


with that said, I will answer OP's question.

OP wants to do "Flash" chromatography, which is a bench-top procedure that is used all the god damn time in chemistry labs of all shapes and sizes all over the world. easily the most common method of chromatographic separation.

it requires a relatively large amount of solvent. it is also very sensitive to the amount of material you are trying to separate. 10 grams is about as much as you could ever separate using flash chromatography.

most people separate about 500 mg to 1 gram at a time (maximum). They do make columns designed for larger loading, but they are hilariously large. 10 gram column loading will require a column with about a 10" diameter (they call them "horse dicks" or "donkey dicks" because they are soo big). these are usually also at least 2 feet in the length of the main column section.

you need somewhere in the neighborhood of 0.5 to 1 mL of dry silica per miligram of material to be purified... this is a very general rule of thumb, and some labs use a different metric. it depends on what and how much you are purifying. keep in mind, "donkey dick" columns can hold about 20 liters (pi*(12 cm)^2*50 cm volume ~ 22 liters).

when you buy silica, as a researcher, you buy big fucking barrels. literally. big barrel. like 2-3 feet tall, 3 feet in diameter. big gigantic plastic barrels full of the stuff.

most O-chem labs have MANY MANY of these big barrels. so that gives you an idea of how much and how quickly you use this stuff.

basically, if you are going to purify 500 miligrams, you would use 250 to 500 mL of dry silica. if you are going to purify 10 grams, you would want to use around 10 liters of the stuff.

you would then pour hexane into the dry silica to make a "gel" or "slurry."

you put a cotton plug at the spout of the column (the "bottom" where stuff comes out), pour a little bit of sand or sodium sulfate on top... then pour the slurry on top of that.

you then "pack" the column by agitating it, causing any voids or bubbles to collapse, so that the density of the silica slurry is more or less even throughout the entire column length.

people usually achieve this by banging on the column with the palm of their hand (we used to tap on it with our cork-stands). you do this for a few minutes, making sure to get it as even as possible on all sides and parts of the column length.

you then pour sand/sodium sulfate on the top of the slurry to "protect" its surface


now, at this point, you should still have a little bit of solvent visible above the layer of the silica/sand, because you packed it in and so it condensed a little bit. You should push this layer of solvent down to just barely above the silica/sand (the top of the column packing) with the air pressure. do not push it further.

you must obviously have the stop-cock open to allow the solvent to run through, but immediately turn it off as soon as the solvent has been pushed to the correct level.

you then dissolve your mixture (BHO) in the solvent system you will begin with (say, hexane:ethylacetate 75:25 or something).

you then put the air-pressure on to push the visible solvent so that it is JUST BARELY above the surface of the sand/sodium sulfate layer (DO NOT push it all the way into the layer, this "dries" the column and ruins everything).

again, you must open it and close it during this procedure

you then add the first batch of your solvent system to the bulb (most flash columns have a "bulb" at the top, so that you can add enough solvent to keep it going for a while).


you then begin pushing it through and collecting fractions.

Periodically you will have to add more solvent.



so if you do the math, purifying 10 grams of material with flash chromatography is expensive as hell. In solvent and silica alone, I am thinking something like $500 to $1000 for 1 single extraction.

the column would probably cost around $200. and you are going to have a hell of a time evaporating the LITERAL gallons of eluted solvent without a rotovap (which cost around $5000 if you include everything, from the rotating section, to the condenser, to the collection flask, to the vacuum pump)




Chromatography is always expensive and time consuming. When they make drugs on the large scale, they usually try to avoid it, because it is so expensive to use chromatography. Even the most ridiculously huge factory-sized columns can only purify 1-100 kilgrams at time...

any chemical produced on the thousands or hundreds of thousands of kilograms per year scale DOES NOT USE chromatography at any point in its synthesis.


purifying 1 kilogram of material requires a 1-2 foot diameter, 3-4 foot long column at about 3500 PSI or more. its the type of thing that requires a mechanical engineer to design.

[VWFringe]

thank you - very much for following up on this and giving up-to-date info

other than using chromatography is there any other ways to simply remove dye and sugars from QWISO? (using ether, would a process using acid/base to move actives through different fluids work?)

[greyphilosophy]

If you don't know proper lab technique and safety don't attempt any of this. I knew a really smart guy who made a mistake with a solvent that was heavier than air and a burner sitting 20 feet away. He almost blew himself up.

Gordonliu makes a lot of good points. I think however the costs of column chromatography are not as high as his estimates. The solvent that comes out of the bottom of the column can be fed back into the top until one of the layers of your column makes it to the bottom. The rotovap we used in the lab also condensed the solvent after evaporating it so the losses were small.

I haven't actually tried this but I don't see why you couldn't reuse the column after you flush everything through it. I sometimes dream of owning a rotovap. What I would try doing if you're trying to make the purest honey oil you can is soak your cannabis in the solvent, filter out the cannabis, and then evaporate most of the solvent. Then take what's left and place it on top of your column and run the same solvent through. This way you know everything will dissolve into your solvent and your column will be clean when you're done.

I would suggest doing some sort of wash after you make your extract. Some solvents are very harmful, especially when inhaled, so you want to be sure your final product is clean.

I've seen butane extractions produce very high quality oil. I would try butane before chromatography, its much easier to do and since butane evaporates at room temp you don't need the rotovap.