Failed second recrystallization

[Guernica]

I successfully pulled ~10g of impure looking spice with Zippo Lighter Fluid a few days ago. The resulting product was an orange-brown, definitely active, sandy textured substance(powdered bark). I was unsatisfied at this point and proceeded to recrystallize all off it with the same solvent. This went peachy. The resulting product was ~7g of orange(not brown) more crystalline spice. The waste was a dark brown goo at the bottom of of a tall thin glass.

Still unsatisfied.

I attempted to re-x 5g of the spice again(I only had around 1/2C(118ml) of solvent left which added up to a little more than 20ml/g of DMT) to obtain a more pure product, but this is where things got strange. I did the same exact procedure, but the solvent turned a milky-yellow color and tons of crystalline DMT started to precipitate out and descend into the waste which had been collecting at the bottom of the glass as the solvent cooled. I used a baster and then an eye dropper to collect the solvent on top, despite what had just happened. I proceeded to evaporate the lighter fluid and what resulted was nearly nothing, and it looks exactly the same as before. What remains on the bottom of glass I was using to recrystallize looks exactly like what I put in it.

I realize that I can just scrape it out and try again, but what the heck happened? Is this the purest product that I can obtain using this solvent? Living in Southern California, this was the only solvent available to me until this point in time. I have located an art supply store that carries Bestine and I'm going to buy a quart of it tomorrow. Do you guys think using a different solvent will make this any easier/better?

 

[ChemisTryptaMan]

I wouldn't trust lighter fluid. Did you test some of it by evaporating it and seeing if it left any residue? This is a must when trying any new solvent. Bestine will work well but while at the art store check and see if they carry gamsol, it is actually naphtha just by another name. Bestine can be used to pull but is much better for recrystallizing and for pulling solvents like naphtha are better. I have had some spice that had a brown color that would not come out. The crystals all looked perfect except the fact that they were brown. There are some other alkaloids which for some unknown reason will sometimes make it into the product. Yellow coloration is the easiest to deal with IMO, it always seems to come out with a few re-x's. Hope you have better luck with your next solvent.

 

[Guernica]

I tested it and it evaporates clean. No worries there :thumb_up:

I've read that pulling with Heptane typically produces a cleaner product, is this true? I'll look for some Gamsol if not.

 

[Guernica]

The MSDS sheet for my Heptane states 100% purity, but after recrystallizing with it my spice has taken on the distinct smell of charcoal.

I didn't think to evap test it because of the MSDS declaration, but definitely decided to after smelling my product. Slight charcoal smell after seemingly dry, but it dissipated sometime while I was away for a few hours. What do you guys think is going on here? Think my spice is alright?

I left my spice container open while I was away in hopes that the smell would disappear. It's definitely not as strong smelling as before, but the smell is definitely still there.

 

[ChemisTryptaMan]

Sorry for taking so long to respond, busy week. By now I would assume the smell is gone from your spice. If the solvent evaporates cleanly it should not leave anything in your product. I hope this has been your experience. If you are still having problems let me know and I'll do my best to help you out.

 

[ChemisTryptaMan]

Also I forgot to respond to your question about bestine. The answer is that yes heptane does typically pull a cleaner product, but it also leaves more of the spice behind. I find it is better to use a solvent that will pull more of the spice, then clean the product by recrystallizing it. If you want to just pull with heptane, it will work, but you will most likely experience significantly decreased yields. Heptane pulls more cleanly because it has such a limited capacity to solvate the alkaloids. It pulls only a limited amount of spice from the aqueous layer, but also pulls far less of the other stuff that you dont want. IME it is best to always re-x your product at least once, preferably until it is pure white. Even when you have what appears to be white powder a re-x will reveal some dark red/brown gunk and a bit of yellow oil, even when it looks pure from the start. If your going to re-x either way, why not pull with something that is going tyo grab as much spice as possible, and save your heptane for cleaning up your product?

 

[Guernica]

The smell never went away. The Bestine definitely had some sort of impurity in it.

Dissolved the nasty spice in some warm and clean solvent, did a sodium carbonate wash, yield dropped a little, but the spice is clean and beautiful now.