Over 50% Loss by Activated Charcoal Purification

[blue.magic]

After doing the Cyb's A/B extraction Tek with naphtha, I arrived to over 1 gram of crude DMT extract from 250g powdered MHRB.

I redissolved the extract in warm heptane and boiled with activated charcoal, according to the Purification Tek.

When I trasferred the pyrex dish with heptane to the fridge, it crystallized immediately. A big white/translucent crystals grew in just few hours.

Unfortunately, the yield was just 263 mg (0.1%).

When filtering the charcoal, most of the DMT maybe soaked into the coffee filter and stayed there.

I have also bio-assayed the oily residue which was VERY strong!! I am confused - the residue is just as strong as the pure product. I expected its effect will be little to none. I have also treated MHRB with Zinc and de-fatted thoroughly so I expected little to none DMT-n-oxide in the residue (that would cause the effect).

The purification step now does not make any sense to me. Why purify then? Just for the beautiful crystals? To keep the pipe cleaner?

Also why the purification leaves so much product in the residue? Is this how it is supposed to work?

 

[Jees]

... according to the Purification Tek...

They call colored spice having impurities.
Against the color white the yellow spice might look 'impure', but against being-active there's nothing much impure about colored spice. It's the white purists having their party again, they suffer a phobia against all non-white. To each his own, if eye candy is so important then pay a price for it.

A water wash (on the spice laden solvent) with a tiny pinch of sodium carbonate in it is all it takes to wash out traces of real impurities, and gives about zero loss in yield.

 

[blue.magic]

It's the white purists having their party again, they suffer a phobia against all non-white.

The motivation here is not fear of impurities, but to know the exact dose. I don't want to have two yellow-tanned spice batches, one being twice stronger than the other.

Once having 95%+ DMT extract, then when you weight 20mg of it, you know it is at least 15mg of DMT, not like something between 1-10mg.

Thanks for mentioning the sodium carbonate wash - I know about it form the Nexian DMT Handbook but it does not say when it is appropriate or when to do it (before charcoal, after?, do either sodium carbonate wash or charcoal or both is best or does not matter?) ... there are still too many questions. But what I need is a reasonably pure product so that specific amount of it gives consistent results.

Various teks I've read contained a chapter about purification, so I came to conclusion it is somehow important, though no author said why.

It's because it will be given to a friend and I don't want to disappoing him if he takes 30mg of it and feels it like 10mg because of the impurities...

 

[Jees]

All the yellow is active, not inactive. Same power as the white. No worries.

 

[concombres]

It's the white purists having their party again, they suffer a phobia against all non-white.

The motivation here is not fear of impurities, but to know the exact dose. I don't want to have two yellow-tanned spice batches, one being twice stronger than the other.

Once having 95%+ DMT extract, then when you weight 20mg of it, you know it is at least 15mg of DMT, not like something between 1-10mg.

Thanks for mentioning the sodium carbonate wash - I know about it form the Nexian DMT Handbook but it does not say when it is appropriate or when to do it (before charcoal, after?, do either sodium carbonate wash or charcoal or both is best or does not matter?) ... there are still too many questions. But what I need is a reasonably pure product so that specific amount of it gives consistent results.

Various teks I've read contained a chapter about purification, so I came to conclusion it is somehow important, though no author said why.

It's because it will be given to a friend and I don't want to disappoing him if he takes 30mg of it and feels it like 10mg because of the impurities...

Try out your product at different stages & purify if the potency is not at a level you are comfortable with.

Sodium carbonate wash after pulling but before freeze precip. After you freeze precipitate all pulls, combine & recrystallize if you feel inclined. For me, as long as it dissolves in a small amount of warm, not hot, WARM solvent without leaving a visible oily or gooey substance in the container, it is pure enough that it needs no further cleanup. Sometimes there is some yellow that is not noticably any more or less potent than the white fluffy crystal.

Personally if i were sharing an extract with a friend, i would let them know there are multiple grades of product that can be had, alot like marijuana concentrates, & they can try different kinds & see what they like best.

Also, that clear oily residue the crystals from recrystal grow on top of, if that is what you are referring to in the post above, i believe to be high quality DMT, just precipitated real fast by the temperature change so no real crystal structure. The more extraction you do the more you will notice during pulls & recrystallizations that the crystals always seem to grow out of this stuff. Otherwise they would not stick to the glass.

 

[Jees]

Blue.Magic read this:
red yellow white spice whats the difference?

 

[blue.magic]

Okay thanks for all the valuable advice.

I wonder what the weight difference is between yellowish extracted DMT and pure DMT. If it's just 0.1% or so, than it does not really matter.

The problem is that a friend of mine requested 1 000 mg of DMT. I don't want to give him 1 000 mg of extract, which may have just 400 mg of DMT in it. I would like to really give him the proper amount.

if that is what you are referring to in the post above, i believe to be high quality DMT, just precipitated real fast by the temperature change so no real crystal structure

Yes what I got were not big "crystals" but neither just white flakes. It is glittering clumps of semi-transparent white and it is pleasurable just look at it - like ice particles on snow.

Unfortunately, it is contaminated with charcoal particles (as I don't have a good filter yet) so it looks bit like salt and pepper. I just hope the charcoal is not a problem for vaporization...

 

[Jees]

...Unfortunately, it is contaminated with charcoal particles (as I don't have a good filter yet) so it looks bit like salt and pepper. I just hope the charcoal is not a problem for vaporization...

STOP. Please.
Never start out with contaminated product.
You don't want a pipe or whatever combusting charcoal at such a moment :shock:

BTW I wonder why you want to hand out something you have no experiential hold on. This really sounds not okay to me, it feels forced. Give yourself time to cross the full learning process and a 'friend' expecting you to come over with 1 gr of spice is a red flag in my book.

 

[blue.magic]

BTW I wonder why you want to hand out something you have no experiential hold on. This really sounds not okay to me

I tried it several times myself without problems. It is to be used in a vaporizer, not in a pipe! The charcoal is just a few very very tiny particles and its an organic (food grade) charcoal and I doubt it would ignite in a vaporizer (even if so, the amount is negligible).

Me and my friend are experienced in psychedelics, we attended meditation retreats together and he as an experienced therapist. I know him for years. We both also did several ayahuasca sessions.

Please don't judge before you know the facts.

And of course I will ask him why he needs a gram of DMT, what purpose it is for, what are his expectations etc. He does the same whenever he gives someone a drug.

 

[blue.magic]

Anyway, my original question was why 50% loss due to purification.

But the answer is probably because the other half was left in the residue (since it is as potent as the "purified" stuff - to my amazement) and some DMT was probably lost in the coffee filter (soaked in with the solvent). I will NEVER use coffee filters again and wait for the vacuum filtration device. No more loss of the priceless product.

 

[Jees]

...Please don't judge before you know the facts...

More power to you both having plenty of experience, I tip my hat for that.

I had a judgement about your extraction experience, that is true.
I'll bent that into some trust from here on

 

[Mindlusion]

I have also bio-assayed the oily residue which was VERY strong!! I am confused - the residue is just as strong as the pure product. I expected its effect will be little to none. I have also treated MHRB with Zinc and de-fatted thoroughly so I expected little to none DMT-n-oxide in the residue (that would cause the effect).

The purification step now does not make any sense to me. Why purify then? Just for the beautiful crystals? To keep the pipe cleaner?

Also why the purification leaves so much product in the residue? Is this how it is supposed to work?

basically yup

there are a lot of threads on this, a recent one popped up a couple months ago

for the most part you can even get beautiful white xtals without the use of AC because the yellow oil falls out before the crystals form.

you should not use coffee filters and you should use celite to remove the AC. Indeed yellow oily dmt is still something like 97% DMT, it only takes a little bit of impurity to prevent crystal formation

 

[pitubo]

I second Jees' sentiment. Admittedly without really knowing the facts, I nevertheless get a distinct impression that the issues presented are commerce related. Gifting a friend should not involve "1.000" gram and the gift wouldn't have to look like glass shards. A safe and satisfying gift should suffice.

I hope you understand and respect the concerns forum members feel about possibly sales related talk.

 

[blue.magic]

Gifting a friend should not involve "1.000" gram and the gift

Disclaimer: I am strongly against any selling. I am pro harm reduction and I have seen people hurting themselves for example by eating impure MDMA (which was mostly MDA). I know how impure product can harm and I don't want to do that to my friend as I am new to extraction and this DMT realm. So better be safe than sorry.

I wanted to remove traces of lye or any chemicals to give my friend a pure smooth experience. I was afraid the impurities would cause caughing, harshness, nausea etc.
That's why I bother with (expensive organic) activated charcoal and the washing steps...
Another reason, as I said was that I was afraid impure product would be weaker (which proved itself false later).
I was a bit paranoid about the impurities - I thought they are problematic and decrease the quality noticeably.

I even use vacuum dessicator to remove traces of solvent from the product. The other purification steps are there to remove traces of zinc and lye. I want to give my friends something extraordinary, something they can't buy.

I also love the lab work and making nice stuff. That's my motivation, I cannot do it without the beauty/purity aspect.

 

[blue.magic]

you should not use coffee filters and you should use celite to remove the AC.

Thanks for the advice. Is it possible to use standard silicagel powder instead of Celite? I can acquire it but it is sold only in large amount or expensively from chemical supplier.

 

[pitubo]

I am strongly against any selling. I am pro harm reduction

I see no reason to further doubt your statement of clarification. All I wanted to point out is how your initial descriptions might have caused eyebrows to be raised by some of us.

I wanted to remove traces of lye or any chemicals to give my friend a pure smooth experience. I was afraid the impurities would cause caughing, harshness, nausea etc.

Any impurities like lye and plant solids can easily and effectively be removed by recrystallization. Simply redissolve in warm clean naphtha. Let this stand for a few minutes in the same warm water bath that you used to warm the naphtha in then and carefully decant from the insoluble impurities into a clean freeze precipitation container. A slower cooling trajectory will yield bigger crystals and thereby better purity.

If you insist on filtering then consider this: After you have filtered a solution containing dmt, flush the filter with warm clean solvent and add this to the solution. I would think this is pretty self evident lab technique.

Lastly, I personally doubt that impurities are the main cause of harsh smoke. Rather, bad smoking equipment and bad smoking technique are the main causes of these problems. Really, instead of investing so much time and money into refining your dmt, you should invest in good smoking device and (even more important imho) good smoking technique. Then pass this knowledge to your friend. Allow for a bit of a learning curve, both for yourself and your friend.

Good luck and safe travels!

 

[blue.magic]

Thanks. I think it's all clear now.

I prefer GVG but even oil pipe provided smooth vapor so I am now quite confident in the product.

The friend wanted 1 gram because he was also afraid of impurities and thought he require much more for several doses. After explaining him extracted DMT practically as potent as pure one (extremely potent), he is happy with 200 mg gift which will serve him many travels.

I will definitely teach him how DMT is different to other substances and how to vaporize it properly.

Sorry for probably reiterating the basic issues, I came across them even after hours and hours of studying teks and forums. It seems I learn mostly by trial and error.

Any impurities like lye and plant solids can easily and effectively be removed by recrystallization.

I somehow felt that even after re-x, the impurities will fall on the crystals (especially lye, which is polar and therefore - I guess - insoluble in NPS) in the end anyway hence why I was so into filtration.

 

[Mindlusion]

you could use silica, it might not catch all the AC though, unless you sucked it through a plug of silica with a vacuum

just buy the diatomaceous earth ant killer at the hardware store, its the same thing as celite

 

[someblackguy]

Very little activated carbon is needed to remove the colored impurities from a solution. You must be careful in your use of decolorizing carbon: if too much is used, it can adsorb the desired compound from the solution as well as the colored impurities.

"adsorb the desired compound"? Huh, so I guess it can...

My first inclination was to redissolve your residue in a small amount of acidic water (fumaric, citric not acetic acid) then add a larger volume of 70+/-% IPA, filter, then evap the liquid. But it turns out that's not the only or the best route.

This thread might be useful: Activated Charcoal (2011, Advanced/Enhanced chemistry)

add your slightly acidic [aqueous?] solution into the AC [containing alks?], then wash the alks out with ammonia in a primary alcohol.

Okay that's what I thought at first (minus the ammonia/base). I can't speak for the authors but I think that the reasoning is something along these lines...

AC/charcoal is a non-polar adsorbent—I mean that it selectively (or preferably?) adsorbs/removes non-polar compounds—lipids, volatile oils, freebase alkaloids—from SOME solutions:

activated carbon is useful for retaining bulky molecules (which chlorophyll is) and nonpolar molecules

Alrighty. Apparently the binding is less specific than I understood it to be, owing not just to ion exchange but multiple phenomena:

the adsorption is not unlike nonspecific binding encountered in various [protein] chromatography methods, it's predominantly van der wahls interactions; no match for dcm, chloroform, or acetonitrile.

*edit* actually, ammoniacal methonol or ethanol would elute it and leave behind fats and other nonpolar compounds

m'kay... So to remove the (freebased) actives from the AC elute/wash it with an organic solvent? Not acidic water like I first thought... my idea might leave the non-polar junk in the resin, but it would likely cause a mess that's a pain to filter. A US Patent filed in 1993 concurs:

US Patent No. 3631059 discloses a process where the alkaloid is extracted from the plant material by using a diluted aqueous solution of a strong mineral acid or a strong organic acid, neutralizing then the acid aqueous extract to a pH between 5 and 13 and adsorbing the alkaloid on activated carbon, separating the carbon by which the alkaloid has been adsorbed from the exhausted solution and finally eluting the alkaloid with an aqueous solution of a strong mineral acid or a strong organic acid. In this type of process the aqueous extracts resulting from the extraction with diluted acid solutions contain various types of impurities coming from the plant (chlorophille and other pigments, sugars, starch, proteins, tannin, fat, etc.) which cannot be removed either by filtration or by strong centrifugation. Such impurities lead to a quick exhaustion of the carbon and also, after the alkalinization, give rise to stable emulsions which make extremely difficult the subsequent phases of the process. In the last analysis, the process according to the above mentioned US patent, though providing an alternative to the use of organic solvents for the extraction of alkaloids from plant tissues, is however not workable in practice due to the above described incoveniences.

"not workable in practice"? Huh, I guess it's not.

Also why the purification leaves so much product in the residue?

For the sake of removing "impurities," it would seem the degree to which AC binds to any compound depends on the solvent, the temp, time, agitation, the compounds in question, as well as the concentration of AC.

I would use this method:

The activated carbon [your resin] is then shaken with a little more fresh solvent [your heptane, ethanol, DCM], and filtered again. Combining both filtrates.

Here are some potential alternatives to AC (recommended elsewhere on the Nexus in regards to Purification Tek)

Celite, diatomacious earth, and silica gel are all forms of silicon dioxide. Mentioned in a previous post each with slightly different applications, composition, and structures.

Bentonite, fuller's earth, kaolin are forms of aluminum silicate which are similarly used as adsorbents.

Alum (alumimum sulfate, aluminum hydroxide) I have used alum with some surprising results. Check out this US Patent Process of extracting, purifying, or excluding alkaloids and alkaloidal salts.

[off topic: Obviously the total amount of adsorbed compounds can vary from one solvent to another. So does it stand to reason that the ratio of one compound (say dmt-oxide) versus another (DMT) adsorbed to AC can depend on the solvent system too? For example, if AC filtered from your heptane and eluted (again with heptane) and dried is 50% lipid, 30% dmt-oxide, 20% plant rosins 5% dmt, might DCM or ethanol treatment yield 80% DMT, 10% fats, 10% etc... when eluted/washed out of AC and dried? Okay it almost certainly does vary, but would that difference between the two samples vary significantly enough to matter for this purpose?

 

[blue.magic]

Thanks for the elaborate answer and the fresh solvent tip, it's certainly an improvement to the process.

I've read on several places on the forums that the loss after purification was about 10%, so I expected that and was shocked when I lost over 50%.

My best guess is that most of the product must have soaked in the coffee filter (never use coffee filters!). I will use only small circular filters with Buchner funnel and wash them after filtering. I don't blame the AC because I have used just a very tiny amount, less than a speck. It would certainly not be possible for it to eat up 200 milligrams worth of alkaloids.
After pouring warm saturated heptane solution, I saw how much product got stuck on beaker walls - so washing is absolute necessity to avoid loss.

I will weigh the purified product plus the residue and compare it to the crude extract. I guess the loss will be much smaller when proper filtering is used.

I am still looking for a good literature on general alkaloid extraction as it should also cover proper purification steps before - say - column chromatography. I found interesting literature on HPTLC analysis of plant alkaloids but it's a long run. A kind of side project.

My current process is the following:

1. combine naphtha pulls
2. wash naphtha with warm sodium carbonate solution (first purification)
3. freeze precipitate, scrape crystals, dry
4. elute in warm heptane, decant clear heptane from residue
5. boil clear heptane with very little AC (second purification)
6. filter (enhanced with Celite)
7. wash filter with more heptane
8. recrystallize, scrape crystals, vacuum dry

It worths to note that this is really not necessary as my product is very pure and usable as is. However, my goal was to get nice crystals and gain more alkaloid purification practice.