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benzyme
#21 Posted : 2/13/2012 12:34:32 AM

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if it's "evaporated", it's technically boiled off.
I've done it, and it recrystallized. I've never seen this black residue you speak of,
that doesn't sound like DMT.
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 

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gibran2
#22 Posted : 2/13/2012 12:53:25 AM

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benzyme wrote:
if it's "evaporated", it's technically boiled off.
I've done it, and it recrystallized. I've never seen this black residue you speak of,
that doesn't sound like DMT.

Well, then my terminology is incorrect. Or are you suggesting that “boiling off” can occur below the boiling point?

On a cold dry winter day, ice will “evaporate”. Substances do not need to be at their boiling point to dissociate and enter into the atmosphere.

If you heat most organic compounds sufficiently, they will break down chemically, won’t they? Why would it be surprising that DMT can break down when exposed to excessive heat for a sufficient period of time?
gibran2 is a fictional character. Any resemblance to anyone living or dead is purely coincidental.
 
TmC47
#23 Posted : 2/13/2012 12:55:01 AM

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Istubar wrote:
After reading a lot of information, I did more steps in my research, but I still having questions.

Seems that the method that adjust to my ideas is STB. I will have 50gr of Mimosa, and if I'm not wrong, that means a proportion of 50gr of NaOH, and 750ml or 1250ml of water (the first volume according to de 15ml rule, and the second according to the molarity).

Then I should do the nexts things:

1) Mix H2O + NaOH + Mimosa, shake well and let the mixture take some time in the container (the more time the mixture rests, better results)
2) Then, add the pentane/naphtha (as desired) to the previus mixture
3) Very soft shake or removing the mixture with something, in order to avoid non desired emulsions, and like #1, let it rest
4) Separate the mixture and use the one who has pentane + dmt, using a filter. Discard the darker with remains of NaOH and mimosa
5) Move the filtered liquid to another container, and put it into the freezer
6) Wait until the cristals appears, and scratch them

And my questions are:

- Are the proportions of each thing right?
I would go with 750 ml of water to 50 g of lye. 50 g of bark is not a lot, and lye that is a bit stronger will break down the cells of your mimosa better.

- In step #1, How many hours do you recommend?
As many as you have patience for. I'd go with two at least, but a whole day is better. Make sure you reach the 5 day mark in the end with at least 3 pulls. 5 is better.

- In step #2, How many ml of pentane? (and how many hours of resting too)
I have no experience with pentane. Isn't that a refrigerator coolant? That would mean it's pretty volatile. Stay safe, ok? Especially with contaminants that might be in it if it is an industrial quality you're using (like anti-corrosives). If you have a liter of volume of bark-soup, I'd say 50 ml per pull would be enough if the extracting powers of pentane were comparable to those of the other solvents used here. For time, see you second question and my answer.

- After filtering the liquid with a decant funnel, I was thinking on using a kitasato flask with carbon filtered paper in the funnel (because it filter xylene, benzene, toluene and other small organic molecules), to make it more pure and avoid contaminations. Is this a non sense idea? (like the distillation Laughing ) Or on the contrary, This one finally has sense?
I am not familiar with the name 'kitisato flask', but if you're talking about activated charcoal (Norit): I've heard of it being used. But if your going to freeze-precip, there's really no need and you risk a *big* loss of product with the 50 g of bark you're using. I'd say don't do it. And if you feel you need to because you have a solvent of a questionable origin, don't use that solvent!

- How many hours should the liquid spend in the freezer? Is better freezing than evaporating, isn't it?
At least 24 hours, and try not to peek. Try to evaporate to a volume like the weight of your bark in grams: that's 50 ml in your case. And I mean first, BEFORE you put it in the freezer. If you have too much solvent, there is more DMT in your solvent than you can get out like this. That's with naphta, however. Pentane could be different. And remember: Pentane has a wide range of concentrations where it is explosive, and your refrigerator as an electric light that switches on with a contact that is also in you fridge. One spark and your family will have to scrape you off the wall. The freezer usually does not have such a light.

- I think that with this wouldn't be neccesary one afterwash of the cristals, Or do you recommend it? Which thing is better, limonel or sodium carbonate? Does the afterwash reduces the amount of DMT?
If you freeze precip, no wash is neccesary.


- Do I forgot something?

Yes, you have: Dear Istubar. If you are not so 'at home' with chemistry, and not so confident in your abilities as a kitchen chemist, then why would you try to go an untested route by using Pentane? You're really making things more difficult and dangerous for yourself here. Buy Naphtha! In any outdoor/camping shop they sell Coleman fuel. Use that instead of pentane, please.

Thank you very much for your patience Embarrased


YW!
Peace!

benzyme wrote:
you're preparing drugs, not salad.
 
benzyme
#24 Posted : 2/13/2012 1:31:47 AM

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gibran2 wrote:
benzyme wrote:
if it's "evaporated", it's technically boiled off.
I've done it, and it recrystallized. I've never seen this black residue you speak of,
that doesn't sound like DMT.

Well, then my terminology is incorrect. Or are you suggesting that “boiling off” can occur below the boiling point?

On a cold dry winter day, ice will “evaporate”. Substances do not need to be at their boiling point to dissociate and enter into the atmosphere.

If you heat most organic compounds sufficiently, they will break down chemically, won’t they? Why would it be surprising that DMT can break down when exposed to excessive heat for a sufficient period of time?


most organic compounds, particularly small molecules, boil before they dissociate from excessive heat or ionization, unless you combust them. heat-labile compounds, such as proteins, decompose.
obviously, bubbles will appear on the liquid-atmosphere interface when a compound reaches its boiling point with applied heat. I've seen this with DMT, and watched it solidify as crystals, at atmospheric pressure.

and I wasn't clear either, of course volatiles can evaporate off below their boiling point
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
Istubar
#25 Posted : 2/13/2012 1:48:39 AM

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Wow, thank you!

The total amount of MHRB would be 100g, but I would do two extractions of 50g because I'm not sure about the size of the containers (How many ml of water will you use with 100g? The double?). Oh, and I forgot it. How many ml of solvent? In most of the recipes you can read, you have inaccurate quantities. It depends on the PH? (for the solvent you need to add until you reach 2 or 3, and for NaOH until you reach 11 or 13)

Maybe you are not familiar with that name due to the differents denominations, sorry. Here at Spain we call it kitasato, but with the following url I'm pretty sure that you will understand it quickly Smile

Büchner flask

The activated charcoal will be placed in the Büchner funnel of the Kitasato/Büchner/vacuum flask.

I spent a lot of hours reading about non polar solvents (their compounds, risks, ease of find them, prices...) and I really don't want to use pentane (but if I would, I don't even know where to find it Laughing ). Here it's really hard to find naphta (except if you went to an industry supplier and paid more than 60 bucks for one liter... or if you use zippo or stove fuel). The less toxic, less risky, cheaper, easy to find, and also with strong power of elution is heptane. I read the security advice, and is not too much different from naphta. But in any case, Which is your opinion about this solvent?

For me it's a little bit embarrasing because I'm sure of it will sound ridiculous... But what is or what do you mean with pull? I have problems to translate that term, and the funny thing is, that probably I know what it is but not how it's called.

7 years ago I made some practice in a lab. Today I forgot everything related to mathematics, stoichiometry and formulas, but fortunatly, I did not forget the lab's security rules and procedures Wink . Also I still having in my wardrobe my old lab coat hehe.

Hum, I need a last explanation about the freezing. Correct me if I'm wrong please: After filtering, the final liquid (probably more than >100ml, just for example), should be evaporated until it reach the same proportion of MHRB (1g:1ml) before putting it into the freezer. I am right?

Thank you one more time Very happy
 
Mindlusion
#26 Posted : 2/13/2012 4:18:50 AM

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DMT will precipitate out of your solvent at your ratio

You will get better results evaporating some solvent first
Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
 
TmC47
#27 Posted : 2/13/2012 7:33:47 AM

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hehe, don't be embarrassed man, Your asking for advise and you are obviously concerned with your health and 'doing it right'. If you blow yourself up, *that* would be reason to be embarrassed Smile

The *ideal* amount of water and pentane really depends on a lot of things, but as long as your soup is not too diluted or too thick and you don't do just one or two pulls, you can't go wrong by much. Doubling everything is fine.

One 'pull' is one 'extraction' with solvent; the process from adding solvent to you bark, agitating it, letting stand to let it float to the top, and sucking or decanting it from the bark is called a 'pull'.

Pentane has explosion limits of between 1.5% to 81%. That means that any concentration of pentane in air that is between those two will explode if it meets an ignition source.
The boiling-point of pentane is around the 35 degree centigrade mark. That means that a room temperature, it is already giving off LOTS of vapors.
It also has a lower vapor-pressure than naphtha, meaning it will easily start to 'float' in air.
Combine the three, and you have a potential tragedy waiting to happen, unless you move *all* of you operation outdoors. And even then, it's still dangerous. You're basically working with lighter-gas-refills (that what comes in a metal can). A little less dangerous than that, but treat it the same I say!

Peace!
benzyme wrote:
you're preparing drugs, not salad.
 
Istubar
#28 Posted : 2/14/2012 12:17:01 AM

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I've said before about leaving the idea of using pentane! I won't use pentane! Don't worry about that point anymore Wink

Here I put the information about the three compounds (and after reading that, it's easy to understand why. I hope that this will help the people who have the same questions as me)

Toxicity:

Naphta≤Heptane<Pentane

Boiling point:

Naphta 130/180ºC (depending on the mixture)
Heptane 98ºC
Pentane 35ºC

Steam density compared to air (air=1):

Naphta ~4 (depending on the mixture)
Heptane 3.46
Pentane <2.5

Explosive limit:

Naphta 0.6 - 6.5
Heptane 1.1 - 6.7
Pentane 1.5 - 7.8

Flashpoint:

Naphta 38/60ºC (depending on the mixture)
Heptane -1ºC
Pentane -49ºC

Autoignition temperature:

Naphta 229/260ºC (depending on the mixture))
Heptane 215ºC
Pentane 309ºC

The questions are reducing, but I still having few more or I need some confirmations:

- Will heptane work? In my opinion yes and seems not too much unsafe than naphta, but I'm a newbie and maybe I'm wrong.
- The ratio of the filtered liquid before putting it inside the freezer (evaporating some of it first) it's right? 1ml per each gram of MHRB (1:1)
- What about the vacuum/kitasato/büchner flask and activated charcoal filter for the funnel? Useful or useless? Besides the other organic molecules, will it filter the DMT too?
- Any suggestion about PH? (I think that with the PH will be very easy to know the right amount of ml). According to this erowid recipe, they use 2 for the acid and 11 for the basic mixture. I read more that suggests 3, and 13.

Thank you so much for your patience and your help! Very happy
 
TmC47
#29 Posted : 2/14/2012 8:29:14 PM

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Istubar wrote:
I've said before about leaving the idea of using pentane! I won't use pentane! Don't worry about that point anymore Wink

Oki! Sorry!

Here I put the information about the three compounds (and after reading that, it's easy to understand why. I hope that this will help the people who have the same questions as me)

...

The questions are reducing, but I still having few more or I need some confirmations:

- Will heptane work? In my opinion yes and seems not too much unsafe than naphta, but I'm a newbie and maybe I'm wrong.
Heptane will work just fine. It's just that:
a) it is more expensive,
b) it is more difficult to buy (for most of us)
c) you will have less spice when you are finished, but
d) that spice will be more pure.
So for me, heptane is good only for recrystallizing


- The ratio of the filtered liquid before putting it inside the freezer (evaporating some of it first) it's right? 1ml per each gram of MHRB (1:1)
I've read somewhere on the Nexus that heptane will hold NO spice at -18 *C, so any amount of heptane should do. But if you're using naphtha I would go for half of that, meaning let half of it evaporate outside and then put it in the freezer.

- What about the vacuum/kitasato/büchner flask and activated charcoal filter for the funnel? Useful or useless? Besides the other organic molecules, will it filter the DMT too?
I have not tried. It should work, but you will loose some product. If it's lye or fibres or tannins you're worried about, why not just work clean and precise, dry with a dash of magnesium sulphate and recrystallize using heptane? You will have more spice, more fast and it will be as pure as you need, especially if it's you first batch. Remember you want a nice results. Over-complicating things will diminish your feeling of accomplishment for sure. Once you know how to do it, you can refine your technique. This is my opinion.

- Any suggestion about PH? (I think that with the PH will be very easy to know the right amount of ml). According to this erowid recipe, they use 2 for the acid and 11 for the basic mixture. I read more that suggests 3, and 13.
If you calculate all those different recipes for lye that are around, you'll find they are mostly between 12 and 13. My opinion is that the Erowid recipe is flawed, bless their hearts, but not necessarily wrong.

Thank you so much for your patience and your help! Very happy


Peace, and good luck!
benzyme wrote:
you're preparing drugs, not salad.
 
Istubar
#30 Posted : 2/15/2012 2:56:01 AM

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You are like my personal cooking teacher hehe, thank you! Very happy

It's really funny because here is easier and cheaper buying pure heptane than pure naphta (except if you buy mixtures of naphta, which almost always have a different name. It's really confusing).

What do you mean with recrystallizing? Of course I understand the meaning of the word, but not the process Wink

Dammit, I find somethings really hard to understand. I thought that I spoke enough english... The paragraph related to the evaporations was very confusing for me "...will hold NO spice at -18 *C, so any amount of heptane should do" What do you mean with that? I'm so sorry, but you need to explain it like if I was a retarded or even worse Embarrased . Then 1:0,5+0,5? (0.5 heptane evaporated / 0.5 heptane freezed )

The vacuum flask idea was due to the possibility of eliminating any toxic remains of organic molecules from the solvent (and why not, to clear the dirtiness of the mixture after the decantation). Maybe it would ruin the posibility of reciclyng the solvent, but the liquid which should contains the crystals, should be more pure and less toxic (I think). The main risk is, that maybe it could filter the spice too!

This is the description of the activated charcoal funnel paper:

activated charcoal funnel paper discs, used to eliminate toluene, xylene, benzene and another small organic molecules. Specialy indicated to filter water and to eliminate bad smells.

It sounds good, isn't it?
 
vapormeister
#31 Posted : 2/15/2012 5:04:03 AM
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Im kinda blown away by the fact that he mentions "healthiness" first, then lab matireals,time etc second.yet noone mentioned Q2121s limtekRolling eyes
i would be worrying about lye before solvent.
if not wanting to do a limtek why would you be going STB(the quick method)? if you do an A/B with sep funnel the separation is CLEAR. real easy to get your difference. i reduced mine to where it was so thick (300g to 800ml) so i had to be patient letting the lyewater out of funnel so the remains on glass could drip down. but even at that thickness it was a crstal clear line between the solvent and lyewater.You were mentioning worring about dumping remains. with A/B all the bark is done with harmless vinagar and can be thrown in trash. Your lyewater will actually be good for your drain Pleased So therefore my suggestion is you change your extration method plan.
I found that if you use a BIG stainless mixing bowl for mixing the Limtek that you have enough room to get it to texture 2 easily. I then put it in a smaller pyrex bowl so i have a better view of what my pipette is dong during extraction. I learned to love that method after figuring out i needed a bigger bowl to mix in
 
TmC47
#32 Posted : 2/15/2012 6:13:03 PM

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I have not mentioned Q2121's tek because I have not tried it. Love to, but can't get Limonene for a reasonable price here. If you're remotely careful, lye will not be a problem, health-wise or environment-wise. The use of hydrocarbons is, but then I should also leave my car at the door forever. Besides, I was just answering questions directly, and then because no-one else did.. Smile
But I'm glad you did, VM! I've heard the benefits of Q21's tek are big!

OT: Do read the Nexian DMT Handbook!
It will answer your every question, if you read through it a couple of times!

Peace!
benzyme wrote:
you're preparing drugs, not salad.
 
Istubar
#33 Posted : 2/15/2012 10:24:00 PM

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What a wonderful handbook, it's like the DMT-bible Shocked

Vapormeister, I'm conditioned by the availability of the things needed, and here is not easy to find limonele. So i won't do the limotek. I will do it with heptane.

I have made the following recipe by 10 steps:

1] Prepare the mixture of MHRB, NaOH, H2O (50g, 50g, 1250ml. *I prefer this proportions to keep the molarity. I will see and share the results of it)
2] Shake well, and let it rest (12-24h).
3] Add heptane (125ml)
4] Soft shake or stir the new mixture, and let it rest too (12-24h). If any emulsion is produced, use hot water to heat the container, and be patience until it's gone.
5] Filter the mixture and put the liquid into a decantor funnel. Let it rest inside for a while for a better separation (1-2h).
6] Take the clear liquid, and put back the darker one with NaOH, H2O and MHRB into the first container to recycle it and do more pulls by adding more heptane (125ml), or water if it's neccesary.
7] [optional, but I think I'll do it] Use a vacuum/büchner flask to re-filter the clear liquid.
8] Put the liquid into a tupperware which has lid and move it to the fridge (6-12h) -> freezer (24-48h) -> fridge (6-12h) to crystalize it and to avoid condensation.
9] Drain the heptane (recyclable) and let the rest evaporating.
10] [optional, but I don't know if I'll do] Wash the crystals by adding heptane and water+sodium carbonate (1 part of NPS per 4 parts of alkaline solution, 1:4). Do the same as steps 5, 7?, 8, 9* (Does the heptane would be recycable in this last case?)

What do you think about my little recipe? Any stupid thing I've wrote or suggestion?

I couldn't find any info about the proportions of evaporating before freezing, and if it's really necessary (some teks do, and others don't). Do you think that, in this case, evaporating until it reach 1:1 (50g MHRB:50ml NPS) would be right?

And of course, thank you! Cool I'm finally approaching to the final countdown Very happy
 
endlessness
#34 Posted : 2/15/2012 10:44:42 PM

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If you want limonene, the suppliers posted by dagger from ebay uk here: https://www.dmt-nexus.me...&m=258331#post258331 they deliver to spain.

better stir than shake when mixing layers.

Also that seems like a lot of heptane, if you use that much, pre-evap. The place to check for proportions is the FAQ. If theres any more doubts, feel free to ask. Good luck.
 
Istubar
#35 Posted : 2/16/2012 1:15:57 AM

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Ops, my fault. I didn't read that, it resembles a lot to the wiki and the nexian handbook, but they have different contents. Let's see.

Respecting to the limonene, I posted before that the price of limonene/naphta is more expensive than heptane (in this particular case, more than 4 times the heptane price). I'll try first with heptane. In any case, I'm really thankful for your help and suggestion. Maybe I find it useful in the future. Wink

Thank you then! All my questions and doubts finally solved (I hope). In one or two weeks (or maybe less if I have troubles Laughing , but I don't think so) I would like to post some images about this and the results of my extraction.

Cheers!




 
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