DMT Extraction Washes?

[jason_]

Any thoughts on best method of washing my naptha pulls? I am used to getting relatively clear/slightly yellow pulls, but this time around I'm getting quite bright yellow naptha back and I'd like to clean it up a bit before proceeding...

I do not have activated charcoal available, but I tried a sodium carbonate wash in the sep funnel, but it did not seem to have any effect. My naptha is still quite yellow...

I also have ammonia (powder), so I was considering trying to do a wash using that. What concentration of ammonia solution am I looking for? I'm assuming something like 5-10% by weight? Also, is it best to do a wash on the solvent before freeze precip, or should I gather my crystals and then wash once they are dry?

Ideally, I'd like to clean up the naptha before freeze precip.

Any thoughts, suggestions, or corrections would be much appreciated.

Thanks,
Jason

[jason_]

No thoughts or suggestions for this?

I went ahead and recrystallized in freezer and separated the crystals... they are whiter than I expected from the color of the naphtha, but still a yellow/tan color. Not too bad looking really, but I'd still like to wash.

Will go ahead and try the ammonia solution (5-10%) or can I use the sodium carbonate solution here?

In the future though, is it possible to wash the naphtha before recrystallization somehow? Vovin describes washing using sodium carbonate in his TEK, but it didn't work for me... naphtha was still quite yellow after three washes. I know it can be done with activated charcoal and then filtered, but I have none available at the moment.

Thanks everyone...

-Jason

[beardedlady]

You can get activated charcoal at a pet store. You really don't have a pet store near you? When I don't have any on hand, I freeze precipitate my crystals, filter them out.

I take them all in put them in a solvent-safe vial (I usually get around 2 grams to fit into a 12 ml glass vial. Taking new, clean naptha in a seperate vial, I heat the naptha in a hot water bath, and then drop by drop add the warm naptha to the crystal vial.

Basically you want the crystals to dissolve into as little naptha as you can. So add some warm naptha, cap the vial and shake. Add more, until it's all dissolved up. Then sit this vial in a warm water bath, shaking the piss out of it occasionally. Then allow it to settle standing up.

Once it's settled, I'll have a goo, pieces of grit and hairs and stuff all in the bottom. Carefully seperate the DMT-rich naptha from the goo (leave a little naptha in there) and put it in a different vial. Repeat that process one or two more times to make sure you get the rest of your DMT from that goo.

Then freeze precipitate the DMT solution again, and I'll usually have white or even clear crystal formation. Hope it helps. My favourite vials are the ones that aren't rounded at the bottom but have a v shaped bottom, makes the goo fall into the lowest possible part.

[jason_]

Thanks for the response!

That's basically what I've done so far is freeze precip, redissolve in a minimal amount of HOT solvent and am in the process of slow recrystallization.

As for the activated charcoal- I never thought of a pet store. I've always ordered it from science supply shops... will have look tomorrow.

And- what about the sodium carbonate wash? As far as I can tell, this did nothing... my naptha was still just as yellow after the wash. Is this not a viable alternative to activated charcoal, or am I missing something completely? Or is sodium carbonate simply removing the excess lye and not performing a full decoloration of the solvent?

Thanks again for the time.

-Jason

[real_psily]

Hate to say it but even Wally worl has act charcoal. I have found that sodium sulfate pulls some junk out with the water. good drying agent that acts to pull other trash out to a little. mag sulfate can work to. What about a sat salt solution? None of these will pull out color as well as charcoal, but could help I guess. The stuff is cheap at the local X-mart though.

[Norman]

Originally Posted by jason_

I also have ammonia (powder), so I was considering trying to do a wash using that.

Ammonia powder?
You know that ammonia is a gas and that ammonia solution is this gas suspended in water, right?
You've changed the laws of physics, man!
Whatever it is, don't use it.
NP washes don't clean out yellow gunk which is insoluable in water.
You're on the right track with recrystalization though.
If you can get some heptane (Bestine Rubber Cement Remover), it'll be a lot easier than naptha, though naptha will do fine.

[beardedlady]

Originally Posted by jason_

what about the sodium carbonate wash? As far as I can tell, this did nothing... my naptha was still just as yellow after the wash. Is this not a viable alternative to activated charcoal, or am I missing something completely? Or is sodium carbonate simply removing the excess lye and not performing a full decoloration of the solvent?

I'm in no ways a chemist, so I have no idea what a sodium carbonate wash would do for you.

Another option is for you to convert your DMT back into an acid solution, an do a defatting with your solvent. Remember, when your DMT is in an acidic salt form (probably using muriatic/Hcl acid) it won't get picked up into your non-polar solvent, but fats and tannins and similar impurities will.

Doing the defat should hopefully help you pull out some of these other things in your product that are causing the discolouration. Also, you'll have smaller amounts of fluids to work with this time, so you should be able to seperate layers more accurately than when you initially did you extraction.

I know when I'm extracting a few kilos of rootbark, I have a large quantity of fluids I'm trying to separate layers of, and I totally don't worry heavily about how accurate my work is, I'd rather just get everything done mostly and go through a second time to clean up when it's a lot easier to do.

After the defat, just convert your acidic DMT solution back into basic solution, and add your solvent and seperate layers. Slowly re-crystallize, and hopefully you can make some huge crystal chunks if you have very little impurities left over.

I have a really good organic chemistry book (The Organic Chem Lab Survival Manual 7th edition by Zubrick) that I'll scan to PDF this week when I get a chance. It's got a large amount of information as far as extractions, washes, recrystalization and whatnot, and is written in a manner that makes it really easy to understand, even with no chemistry background. It's a huge section on re-crystallization for working with very small quantities of alkaloids. I'll try to get to it tomorrow for you if possible.

[jason_]

Originally Posted by Norman

Ammonia powder?
You know that ammonia is a gas and that ammonia solution is this gas suspended in water, right?
You've changed the laws of physics, man!

Ha! Ok, further investigation leads me to believe it's actually ammonium carbonate... so yes, something different altogether. It wasn't used however, so all's well there.

Originally Posted by Norman

If you can get some heptane (Bestine Rubber Cement Remover), it'll be a lot easier than naptha, though naptha will do fine.

I did my recrystalization in naphtha, but I do have heptane available as well. It was pretty pricey though and I wasn't sure of the benefit so I didn't pick any up. It seems though that at this point one would be using a very small amount of solvent so that may not be an issue. Can you elaborate on the benefits of heptane over naphtha? Is it just a cleaner solvent or does it offer a higher solubility?

Thanks again for the info.

-Jason

[jason_]

Originally Posted by beardedlady

I'm in no ways a chemist, so I have no idea what a sodium carbonate wash would do for you.

From Vovin's TEK (which is the only place I know that it's mentioned):

This is a somewhat new process that is not found in many of the older tek's. This process will try to remove as many of the foreign chemicals from the naphtha solution as possible. Especially the lye that was added in a previous step. The goal here is to leave only the DMT in the naphtha so that when you evaporate you end up with pure crystals.

Begin by taking about 50 ml of Distilled water and placing it into a flask and adding sodium carbonate to it. Just add a pinch to the water. It doesn't take much. You will only be using this mixture for the first wash. Do not use it for the second and third washes.

A little dab will do yah here, add only a small amount of the water/sodium carbonate solution to your naphtha. If you have 300 ml of naphtha then you want to put around 25 ml of the sodium carbonated water. Mix the 2 together and then place them in a seperatory funnel. Shake the hell out of it this is the only mixing step where the liquids separate almost immediately so no worries about too much agitation. Separate the water from the naphtha and discard the water.

For the second and third washes you want to use only distilled water nothing should be added. 25 ml per wash is sufficient. Perform the same procedure as above. You should not leave the water in the naphtha for too long. This means no sitting for hours letting it 'soak' you need to get it in and out.

After a healthy shaking the water and the naphtha almost immediately separate. Only if all separations were this easy. The water is on the bottom of the funnel.

After 3 washes the naphtha is clear as glass.

So, he makes it sound like it will clear up the naphtha and take out any impurities before recrystallization. Would be a huge help if it worked, since now I'm stuck doing a freeze precip and then collecting crystals and washing/recrystallizing afterward.

Originally Posted by beardedlady

I have a really good organic chemistry book (The Organic Chem Lab Survival Manual 7th edition by Zubrick) that I'll scan to PDF this week when I get a chance. It's got a large amount of information as far as extractions, washes, recrystalization and whatnot, and is written in a manner that makes it really easy to understand, even with no chemistry background. It's a huge section on re-crystallization for working with very small quantities of alkaloids.

Yes! I actually have a copy, thanks to another generous Mycotopia member! It's really a great manual... I've uploaded a copy to this thread for anyone else who's interested:

The Organic Chem Lab Survival Manual

-Jason

*edit- Couldn't get the file to upload to the mycotopia server (too large) linked to off-site file...

[Norman]

Originally Posted by jason_

I did my recrystalization in naphtha, but I do have heptane available as well. It was pretty pricey though and I wasn't sure of the benefit so I didn't pick any up. It seems though that at this point one would be using a very small amount of solvent so that may not be an issue. Can you elaborate on the benefits of heptane over naphtha? Is it just a cleaner solvent or does it offer a higher solubility?-Jason

DMT is actually less soluble in heptane than naptha which is what makes heptane a superior recrystalization solvent. It's a lot more selective too - the gunk is way less soluble so it crashes out way before the DMT. One heptane recrystalization is worth two or three naptha recrystalizations. Evaporates really quickly too.
And you're right, very little is used and of that only what inadvertently evaporates can't be reused.
Be sure to save what gets cleaned out, it's loaded with alks still, among them DMT n oxide.
The problem with NP washes and yellow oil is that the yellow stuff is less soluble in water than DMT so you're going to lose alks as well as yellow. NP washes are good if you're worried about water soluble impurities like lye.

[jason_]

Originally Posted by Norman

DMT is actually less soluble in heptane than naptha which is what makes heptane a superior recrystalization solvent. It's a lot more selective too - the gunk is way less soluble so it crashes out way before the DMT. One heptane recrystalization is worth two or three naptha recrystalizations. Evaporates really quickly too.
And you're right, very little is used and of that only what inadvertently evaporates can't be reused.
Be sure to save what gets cleaned out, it's loaded with alks still, among them DMT n oxide.
The problem with NP washes and yellow oil is that the yellow stuff is less soluble in water than DMT so you're going to lose alks as well as yellow. NP washes are good if you're worried about water soluble impurities like lye.

Thanks, that post clarifies things quite a bit. Much appreciated.

So, the sodium carbonate or activated charcoal wash will likely remove any traces of lye left in the solvent... Then, one could move to recrystallization with heptane to clean and purify the crystals once they are collected.

And what about that ammonia wash? I guess there are just many ways of going about the same thing? But are they necessary or worth doing if one intends to recrystallize anyway?

So, say I collect all the naphtha from all my pulls, evap down to saturation, and freeze precip. Now, I have some quantity of small yellow/tan crystals left on the filter paper. Where should I go from here? Ammonia wash, or skip that and go straight to recrystallization in the heptane?

I guess I'm just looking to find the easiest/most direct method of obtaining as pure a product as possible...

-Jason

[Norman]

Originally Posted by jason_

So, say I collect all the naphtha from all my pulls, evap down to saturation, and freeze precip. Now, I have some quantity of small yellow/tan crystals left on the filter paper. Where should I go from here? Ammonia wash, or skip that and go straight to recrystallization in the heptane?
-Jason

My friend just goes straight to recrystalization and gets glass clear shards in one pass.
The ammonia wash helps a lot if the material is yellow but not oily but it doesn't save that much time over a recrystalization and so many people have problems with it, I've stopped recommending it. It also only washes the surface so if there are impurities that the crystal has formed around, they won't be touched.
If you do the NP wash, keep your pH at 12 or you'll lose significant amounts of product.

[jason_]

Will skip the ammonia wash from now on then.

Good point about watching the pH for the NP washes. Will keep that in mind.

Thanks again for all the help.

-Jason