Best eluent choice?

[fatty lumpkins]

Dear bluelighter, this is swim's first post!

Swim is currently working on an effective way to extract THC that can recycle butane using stainless steel pressure tanks. Until said day arrives swim has been looking toward other cost effective means to extract and isolate THC. His method is this:

From the ground up:
Ethanol preparation:

In a (or several) 2ltr bottles cane sugar is fermented with turbo distiller's yeast. When the fermentation has finished a crude distillation is done to separate the primary ethanol fraction. This ethanol is distilled a second time via fractional distillation with a 300mm vigreux colum to an azeotropic solution. A final distillation is performed over calcium oxide to further remove water. This ethanol will be stored under intert gasses in swim's freezer.

Diethyl ether:

Due to the dangers of ether swim will omit the finer details. swim's preparation of ether is carried on otc via nearly anhYdrous ethanol being refluxed with sulfuric acid under an inert atmosphere with a drying tube. When the reaction is complete swim will distill the ether from the acid solution and nuetralize his final product.

Sulfuric acid:

Swim lives in a location where sulfuric acid is VERY hard to find and incredibly impure. Swim prepares his by reacting calcium sulfate with oxalic acid, filtering, and boiling down to the desired concentration for a reasonably low cost.

Swim can also prepare common nitro alkanes/solvents from relatively simple sources with the only expense of time.

Swim's planned procedure:

Swim was thinking that he or she could use cold nearly anhydrous ethanol to perform a thc extraction from some cannibis leaves to experiment with. Swim heard this to have good results.

Swim's question to the more experienced:

Swim's primary question is what would be the most favorable eluent for a chromotography separation? Solvent choice isn't an issue he is resourceful and greatly succesful at obtaining a pure solvent. Swim has little to no experience with thc and is requesting help from more knowledgeable alchemists. Swim also apologizes for spelling errors, his/her current device is not very interactive with autocorrect.

Swim thanks you all in advance.

 

[PotatoMan]

No swimming here. It's a forum, not a pool.

 

[fatty lumpkins]

Haha yeahh old habbits die hard. I'll try not to.

 

[Thomas Davie]

If possible you want to use a reverse phase column packing material. You can load up your extract in a small amount of petroleum ether, draw that down into the column and then start eluting with a polar solvent to flush away contaminants.

You could then start to elute with an increasing concentration of a polar solvent miscible with pet ether (your choice there are lots). There are miscibility indexes online you can look at if not sure. Eventually you'll force pure THC off the column in ~100% etoh (this is your goal, right?).

Then use rotary thin film evaporation to remove the ethanol and you've got your desired product.

Tom

(cold etho is better than room temperature etoh as you'll be far less likely to extract plant pigments and other contaminants)

 

[fatty lumpkins]

That is what I want. Pet ether has all sorts of different solvents in it, will that effect elution? I can prepare a pure ether in situ.

So I should begin eluating with the most nonpolar solvent I've got and then target thc with an eluent? I like that line of thinking . Sounds like EtOH is almost universally accepted for thc. What about glycerol? It's fairly polar I believe and I dont have to worry about it being hydroscopic.

 

[skillet]

Reverse phase silica is best for really polar stuff, amino acids, peptides and all. Regular silica would be a far better choice for this and much cheaper.

I've been trying to find the eluent they use in those cannatest or whatever kits, they seem to get good resolution of the different cannabinoids on tlc. I'm sure I saw it ages ago but now can't find it.

But it depends how well you want to separate, what scale you want to do it on etc. To get a mixture of cannabinoids and just remove the other stuff, toluene/pet. ether mixtures are probably good.