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TEK Looking for advice/comments on extraction

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grudgemaksimit

Esteemed member
Hi

Using lazyman's/nomans teks since around 2010, I now tried with 100% xylene for the first time. Evap test completely clean, but it takes a long time to evaporate.

I started with 50g powdered (very, very finely powdered!) MHRB, 75g NaOH, 0,5l water and used 20 to 30ml room temperature xylene for the pulls. Got a separatory funnel for separating the xylene more easily.

At this point I'm wondering, would heating up the xylene be beneficial. Also I think I went with too little water, I will try atleast 750ml water for 75g NaOH and 50g MHRB for next batch.

I got some promising early results from the first pulls by evaporating a small amount of xylene on a petri dish, the whole surface area formed a nice collection of snowflakes. I got around 150ml now in the freezer and will see what's up tomorrow, but I'm already looking for things to do better, if there is something obvious I may have missed.

One thing I noticed already is, seems the pulls are a bit oily. Could this be a temperature thing, or perhaps the powdered bark itself? Stored in dark & room temperature in a glass jar for many years.

I'm also keen to try a sodium carbonate wash, but will have to wait a bit to get enough material.

Is xylene ok for getting really pure dmt, as my goal this time around is to figure out a reliable way for me to make really pure end product. While I have made many a succesfull batch, I always have this nagging feeling it could've been a little better. I am very severely hampered by laws and regulations though, regarding what materials (i.e. solvents etc.) I can easily obtain.

Thanks for your time!
 
No need to heat xylene, it's a good enough (and stinky enough) solvent as it is. Also, because of this higher solvent power for DMT, there's no point putting it in the freezer - nothing will precipitate.

Pull your alkaloids back out of the xylene with a mini A/B; evaporating xylene is unnecessary.

You'll get a purer product with a more selective solvent like heptane, which you can use for the mini A/B and/or a re-x. It sounds like you may have to seek out alternatives, but until I know your general location it's hard to comment on what alternatives you might be able to obtain.
 
Transform said:
No need to heat xylene, it's a good enough (and stinky enough) solvent as it is. Also, because of this higher solvent power for DMT, there's no point putting it in the freezer - nothing will precipitate.

Pull your alkaloids back out of the xylene with a mini A/B; evaporating xylene is unnecessary.

You'll get a purer product with a more selective solvent like heptane, which you can use for the mini A/B and/or a re-x. It sounds like you may have to seek out alternatives, but until I know your general location it's hard to comment on what alternatives you might be able to obtain.
Click to expand...
Thanks for the reply and information.

Yeah ok will look into AB. Location is Finland, so probably one of the strictest countries. I'd be able to get some brake cleaners, which looked very promising on the datasheet: C6-C7, but it was an aerosol. Would that still be ok, if sprayed into a different container outside? I'll keep looking tho, there is absolutely no hurry.
 
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grudgemaksimit said:
Thanks for the reply and information.

Yeah ok will look into AB. Location is Finland, so probably one of the strictest countries. I'd be able to get some brake cleaners, which looked very promising on the datasheet: C6-C7, but it was an aerosol. Would that still be ok, if sprayed into a different container outside? I'll keep looking tho, there is absolutely no hurry.
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Proper auto suppliers might be able to furnish you with just the solvent part of the brake cleaner - tell them you already have a spray applicator and prefer to "save the environment" or something. I'll have to brush up on my Finnish, somewhere in my files I even have an old copy of the Finnish dangerous goods transport regulations :D Anyhow, here's a recent mention of brake cleaners, albeit UK ones, in another thread:

Confusion over what naphtha or solvent to use for extraction please help...

Hi all . This is my first post on the forum after say 8 months of using the how to guides when pointed in this direction by a friend. I got given some un labelled naphtha to start of my extractions but now I've tried to purchase some myself. I'm a bit worried about selecting the wrong stuff...
forum.dmt-nexus.me forum.dmt-nexus.me

Some of them might contain butyl acetate, check the label. You can extract with butyl acetate (it smells like bananas!) but, again, freeze precipitation won't work with that one either. If that turns out to be the case for you, I can point you in the right direction with that as well.

Glad to hear you're willing to take your time with this, too.
 
Transform said:
Proper auto suppliers might be able to furnish you with just the solvent part of the brake cleaner - tell them you already have a spray applicator and prefer to "save the environment" or something. I'll have to brush up on my Finnish, somewhere in my files I even have an old copy of the Finnish dangerous goods transport regulations :D Anyhow, here's a recent mention of brake cleaners, albeit UK ones, in another thread:

Confusion over what naphtha or solvent to use for extraction please help...

Hi all . This is my first post on the forum after say 8 months of using the how to guides when pointed in this direction by a friend. I got given some un labelled naphtha to start of my extractions but now I've tried to purchase some myself. I'm a bit worried about selecting the wrong stuff...
forum.dmt-nexus.me forum.dmt-nexus.me

Some of them might contain butyl acetate, check the label. You can extract with butyl acetate (it smells like bananas!) but, again, freeze precipitation won't work with that one either. If that turns out to be the case for you, I can point you in the right direction with that as well.

Glad to hear you're willing to take your time with this, too.
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I think I might've found a good one. Brake cleaner from a car supplies store. Says it's 100% on the datasheet and cas search gave this:
Screenshot_20240701_165923_Chrome.jpg
 
Yep I'll give it a test if evaporation is ok, after I'm done with my current pulls with xylene. Just gonna do one or two more and then mix a fresh batch of powder + naoh water to sit and brew for a while. I dont want to work with too many different things at the same time. Will report back in a day or two.
Thanks for your help!
 
grudgemaksimit said:
Yep I'll give it a test if evaporation is ok, after I'm done with my current pulls with xylene. Just gonna do one or two more and then mix a fresh batch of powder + naoh water to sit and brew for a while. I dont want to work with too many different things at the same time. Will report back in a day or two.
Thanks for your help!
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Brake cleaning fluid is specifically intended to evaporate without leaving an oily residue and this constitutes a critical use case, making it idea for 'us' at the same time. But it's still wise to perform an evaporation test - just be aware that traces of grease and detergent must be removed from the test surface beforehand to avoid an annoying false positive result. Use a bit of the solvent on a clean paper tissue for this, followed by wiping with a dry bit of tissue.
 
Evap test was ok so I moved on to use the brake cleaner only. I decided to just evaporate the xylene as there wasn't a lot of it, just a small test so I didn't want to bother with A/B as it would mean more steps and more different chemicals to obtain. It left a lot of yellowish oily goo, and not a lot of crystals, so I was wondering if I could still try to separare some crystals from it by absorbing it into the other solvent?
Anyway it is not a significant amount so it's ok either way.

I now have 3 containers with a few pulls made with the brake cleaner solvent. One container straight to freezer, one partially evaporating and then moved to freezer, and one fully evaporating. I made a couple of the pulls with room temperature solvent and a couple where I warmed the whole soup to 35-36° celsius (approx. 100° F).

I also made 2 different soups, one 50g mhrb and 750ml water, the other with 75g mhrb and 1125ml water. All pulls made with 20-30ml solvent, except one with a lot more, 100ml.

But I never really had trouble with pulling, it's more the purifying part that I can't seem to get quite right. I'm always left with some oily substance (dmt-N-oxide, so its safe, atleast I'm pretty sure that's mostly what it is, because it has a small effect too. I've also had some traces from the naoh soup, very harsh smoke, but doesnt vaporize in normal use) in the crystals, as evident when smoking it. Not a lot and it's not really a problem experience-wise, but still I would like to learn to get rid of it.

Edit: spoke too soon about the xylene, it's actually still evaporating and started to form crystals! Will give it some hours under a fan

Edit2: Initial results of small pulls with brake cleaner look to be very promising. Much whiter spice from the get-go than any solvent I used before over the years, so it is for sure more selective.
 
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Great stuff! Sounds like you're well on the way to cracking this nut.

It has been more or less established that the coloured, oily, active material consists of oligomers/polymers of DMT formed by electron transfer between the pyrrole rings of DMT molecules. Electron loss is another form of oxidation, so "oxidised DMT" doesn't necessarily equate to the N-oxide. The oligomerisation tends to be promoted by longer contact times with the alkaline solution. Thanks to work done by @Loveall, we know that one of the things a mini A/B does is to break up these oligomers to a certain extent, so that you can then, after adding base, use naphtha to obtain white crystals in better yield than would be obtained from the xylene product directly. This is in large part due to the poor solubility of the oligomer in naphtha.
grudgemaksimit said:
Edit: spoke too soon about the xylene, it's actually still evaporating and started to form crystals! Will give it some hours under a fan

Edit2: Initial results of small pulls with brake cleaner look to be very promising. Much whiter spice from the get-go than any solvent I used before over the years, so it is for sure more selective.
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I bet if you tried dissolving the xylene-derived crystals in warm brake-cleaner, you'd be left with a dark, oily blob of polymer. I guess if you did this and separated off the naphtha for recrystallisation, you could then dissolve the polymer in vinegar for a few hours before adding base and doing a couple of tiny naphtha pulls to recover more crystals, which would be much paler if not completely white. Whether you can be bothered to do this largely depends on how much you're interested in comparing the "full spectrum" material obtained with the xylene, versus getting as much 'clean' material as possible.
grudgemaksimit said:
I've also had some traces from the naoh soup, very harsh smoke, but doesnt vaporize in normal use) in the crystals, as evident when smoking it. Not a lot and it's not really a problem experience-wise, but still I would like to learn to get rid of it.
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Besides allowing your pulls to settle in a jug before transferring them to the crystallisation dish, one simple trick is to include a bit of water, brine or sodium carbonate solution in the settling jug. This will help catch stray droplets of lye solution as the naphtha lands in the jug. The water can then be pipetted off before completing the transfer to the freezer - in practice, I've found decanting away from another liquid to be difficult if you don't have a vessel of exactly the right shape.
 
Thanks for the info!

I will let the xylene sit for one more night and see about dissolving the crystals and polymer oil later. It would be interesting to see what happens with it, but I think I'm gonna settle on the brake cleaner for long term.

The warmed up pulls yielded more yellow colored crystals (fresh soup), so I think 36° was a bit too much. I will try lower temperatures to see if I might hit some sweet spot of yield/purity, when I make another fresh mimosa soup.
If nothing else, I will be very happy doing several small (30ish ml) room temperature pulls per small soup batch (50-75g MHRB), if it means more purity.

I'm gonna spend a few days just doing pulls to get more material that I can try the sodium carbonate wash and other purifying methods with, so I will report back when I start that process.

Thank you very much for your time.
 
I've been doing pulls with alternating temperatures, and it seems room temperature is the way to go. Less yield but more initial purity. Need to do more pulls, but it's well worth it. I tried around 30°-37° range, mixing jar in water bath.

For some of the pulls I tried having sodium carbonate water in separation jar and pouring from that through cotton to the jars going in the freezer. This seemed to work quite well in terms of initial purity. I also did a defat for the powder with mixing it a couple times and around 5 minutes at a time in solvent and using a coffee filter to get most of the solvent out, this solvent was discarded as waste material and not used in anything else

Now I'm dissolving some of the material pulled with xylene (which was surprisingly quite a lot!) in 10% vinegar (pH 3-4), and will then add brake cleaner solvent to separate impurities, after that I will add a small amount of NaOH to basify the liquid and another round of solvent to get the hopefully more clean material out.

I'll move on to re-x and sodium carbonate wash after I'm done with this test.

Edit: I settled on making the soups with 75g MHRB, 75g+ NaOH and 1,2-1,3 liters water. Seems to be a good texture, and also a good amount for the containers/jars/separatory funnel I'm using.
 
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grudgemaksimit said:
I've been doing pulls with alternating temperatures, and it seems room temperature is the way to go. Less yield but more initial purity. Need to do more pulls, but it's well worth it. I tried around 30°-37° range, mixing jar in water bath.

For some of the pulls I tried having sodium carbonate water in separation jar and pouring from that through cotton to the jars going in the freezer. This seemed to work quite well in terms of initial purity. I also did a defat for the powder with mixing it a couple times and around 5 minutes at a time in solvent and using a coffee filter to get most of the solvent out, this solvent was discarded as waste material and not used in anything else

Now I'm dissolving some of the material pulled with xylene (which was surprisingly quite a lot!) in 10% vinegar (pH 3-4), and will then add brake cleaner solvent to separate impurities, after that I will add a small amount of NaOH to basify the liquid and another round of solvent to get the hopefully more clean material out.

I'll move on to re-x and sodium carbonate wash after I'm done with this test.

Edit: I settled on making the soups with 75g MHRB, 75g+ NaOH and 1,2-1,3 liters water. Seems to be a good texture, and also a good amount for the containers/jars/separatory funnel I'm using.
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Thanks for all the detailed data regarding your experimentation and subsequent observations. I wonder if in future you'd try using a little less NaOH to compare the results?

Looking forward to hearing how it goes with the clean-up on the xylene material.
 
Transform said:
Thanks for all the detailed data regarding your experimentation and subsequent observations. I wonder if in future you'd try using a little less NaOH to compare the results?

Looking forward to hearing how it goes with the clean-up on the xylene material.
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Unfortunately I'm out of MHRB so I can't test using less NaOH for now.

First separation/cleaning of xylene derived material was a great success. I first cleaned the low pH vinegar mix with solvent, it took out some of the impurities and did not absorb anything unwanted (evaporated it all to make sure, only a greasy surface was left on the plate). After basifying the vinegar mix, a clear layer of brownish oily material separated to the top and the rest of it became a kind of cloud of milky liquid. First pull was made with quite a warm mix, estimating 40ish° (the added NaOH warmed it up, did not get a more accurate measurement as I did not use a water bath around the jar, also dont have a good thermometer for using straight in the NaOH mix). The solvent pulled quite a lot of fats/oils and end result was yellow. Subsequent pulls with room temperature mix resulted in mostly very white crystals after 20ish hours in the freezer, which is below -20°C. I will evaporate the solvent from the freezer to see how much material did not precipitate out, if any.

Next for the xylene derived material I will try exactly as suggested before, first dissolving in warm solvent, separate oil, oil in vinegar.

I have plenty of yellow material now to start cleaning, what kind of re-x process do you suggest? Previously I have tried dissolving in warm solvent and separate from any oily/fatty substance not absorbed, then just freeze and try to separate whiter crystals. I did not do a wash, or pour through cotton, and I was never quite happy with the results. Probably used too little material and too much solvent, and too warm.. just a guess.

This time I was thinking of first dissolve in solvent, then sodium carbonate wash, freeze and then start re-x process after I see what comes out of that.
 
Just bear in mind that DMT is polymorphic and one of those polymorphs is simply yellow in tone. Like these:

Can xylene pulls can be backsalted?

Hey folks please help me on this one as i am wondering, can my xylene pulls be backsalted? Do i understand correctly that i can use water with citric acid to backsalt my xylene, and later add the base solution and do the pet ether pulls to freeze precip my xtals? And how to do it corectly? If i...
forum.dmt-nexus.me forum.dmt-nexus.me
 
Transform said:
Just bear in mind that DMT is polymorphic and one of those polymorphs is simply yellow in tone. Like these:

Can xylene pulls can be backsalted?

Hey folks please help me on this one as i am wondering, can my xylene pulls be backsalted? Do i understand correctly that i can use water with citric acid to backsalt my xylene, and later add the base solution and do the pet ether pulls to freeze precip my xtals? And how to do it corectly? If i...
forum.dmt-nexus.me forum.dmt-nexus.me
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Yeah I'm keeping the yellows and whites separate and will also be purifying separately and not all at once. I guess only way to be sure there are no fats/oils/plant material or other impurities is to just put some in pipe, vape and see if it leaves anything behind?
 
grudgemaksimit said:
Yeah I'm keeping the yellows and whites separate and will also be purifying separately and not all at once. I guess only way to be sure there are no fats/oils/plant material or other impurities is to just put some in pipe, vape and see if it leaves anything behind?
Click to expand...
MHRB extracts, in the context we're working with them, contain virtually no fats or oils. Oiliness is pretty much entirely down to oligomers and polymorphs.
 
Transform said:
MHRB extracts, in the context we're working with them, contain virtually no fats or oils. Oiliness is pretty much entirely down to oligomers and polymorphs.
Click to expand...
Ok good to know, so whatever oil is left after re-x, from whichever solvent derived material, I can try to put in vinegar for a few hours and try pulling a bit more after basifying it?
 
Ok so I did two recrystallisations:

1.
-0,5g yellow/darkish yellow crystals dissolved in warmed up 20ml solvent (brake cleaner, temperature just a shot in the dark, hot water bath with no thermometer, I dont have one atm that goes above 50°C). Some copper colored oil was not absorbed, and was left behind on next step.

-poured into room temperature sodium carbonate distilled water, carefully so no copper colored oil came with it, and thoroughly stirred/shaked. Probably a mistake, should've warmed up the water too, but hey let's remember next time.

-separated, cooled to room temperature

-fridge, 4°C 1 hour

-freezer, colder than -20°C 24 hours

2.

-0.5g crystals dissolved in warmed up solvent like above

-no wash, cooled down same as above and same time in freezer.

Method 1 yielded some pretty white and bigger crystals, but most is quite oily and yellow.

Method 2 no white crystals at all and quite oily.

So the wash definitely helped, but I think the solvent was too hot on both methods, and also the sudden cooling down by the room temperature water probably was not optimal..

Will try much lower temperature next and will start by first warming up 10ml solvent and then add the crystals little by little until they are not dissolved. Also warming up the wash water at the same time.

Will do 2 methods again, one with wash one without.

Edit: added pics
1.
1000023118.jpg
2.
1000023119.jpg
 
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