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DMT distillation Options
 
Istubar
#1 Posted : 2/10/2012 10:21:49 PM

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Hi everyone! Very happy

I'm a full newbie here, so please, have some patience with me (I hope that my english would be good enough to be understood too Confused )

I've started my path to obtain DMT weeks ago, and I think I almost reached all the information needed to start with it, but I read something different and I would like to share it with you to hear you opinion because I don't know if it would be a waste of time and money, or if it would work (I didn't find anything similar in the DMT-nexus wiki and the forum searcher).

Here we go.

I was wondering about the success of distillation DMT doing the following procedure:

We need to start with a disolution of water + NaOH + Mimosa hostilis (1L + 40g + 40g, PH 11 or 13?) inside a flask, attached to one Liebig condenser. Due to the boil temperature of water at 100ºC, NaOH at ~1000º and DMT at 60º, we only need to heat the mixture to reach 70-75ºC, in order to boil DMT, but not the water and the NaOH that should remain at the flask.

Then, the Liebig condenser will made his work by freezing the DMT vapour and creating the cristals inside of it. The cristals should be free of any remain of NaOH due to the difference of the boiling temperature.

Would it work or just in my imagination? Do I forget something important?

I prefer this method to extract DMT in order to use Naphta or similar toxic chemicals, to avoid any possible contamination.

Help please!
 

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Mindlusion
#2 Posted : 2/10/2012 10:45:22 PM

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The MELTING POINT of DMT is around 60ºc
Actually it seems to be somewhere between 40C and 50C, I'm not exactly sure, seems there has been debate.

Perhaps it is closer to 60ºC, it seems to vary from different sources from 44C to 68C. Aldrich got values 58-60C and 64-67C


the boiling point of DMT is 160ºC *not at STP*

Twisted Evil
--

Also this method if it were to work, would likely not be effcient or more pure then a non polar extraction, actually it would be less pure because you would also be distilling oils and other volatiles and constituents of the root bark.
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geko42
#3 Posted : 2/10/2012 11:04:56 PM

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very interesting thought, but mind has a good point you would rely want to know the boiling point of the other impurities, plant fats and what not.

swim is curious on why not using a non polar extraction? are you just exploring?
 
benzyme
#4 Posted : 2/11/2012 12:50:59 AM

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Mindlusion wrote:

the boiling point of DMT is 160ºC.

iirc, this figure is for reduced pressure. the temp adjusted for 1 atm is 375 C

oh and istubar, that won't work. you're going to have to isolate the alkaloids
before distilling them. don't fear the chems.
"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
 
gibran2
#5 Posted : 2/11/2012 2:23:42 AM

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benzyme wrote:
Mindlusion wrote:

the boiling point of DMT is 160ºC.

iirc, this figure is for reduced pressure. the temp adjusted for 1 atm is 375 C

oh and istubar, that won't work. you're going to have to isolate the alkaloids
before distilling them. don't fear the chems.

And at standard pressure, it would decompose rather quickly when heated to 375°C, wouldn’t it?
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benzyme
#6 Posted : 2/11/2012 2:36:55 AM

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not necessarily
it doesn't have any functional groups that are heat-labile
"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
 
gibran2
#7 Posted : 2/11/2012 3:23:14 AM

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benzyme wrote:
not necessarily
it doesn't have any functional groups that are heat-labile

Then why does it turn golden --> brown --> black when it's heated in a test tube? And why isn't there a B.P. at standard pressure listed anywhere?
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benzyme
#8 Posted : 2/11/2012 4:25:15 AM

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that doesn't sound like dmt. otherwise, how would you be able to vaporize it?
compounds which decompose do not have boiling points. there seems to be a lack of several constants for dmt, but you don't vaporize DMT at 0.8 hPa, do you?

ACD/Labs calculates 332 C at 1 atm

http://www.chemspider.co...ical-Structure.5864.html (properties-->predicted-ACD/Labs)
"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
#9 Posted : 2/11/2012 4:26:16 AM

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Thank you all for your answers Very happy

Mindlusion wrote:
The MELTING POINT of DMT is around 60ºc
Actually it seems to be somewhere between 40C and 50C, I'm not exactly sure, seems there has been debate.

Perhaps it is closer to 60ºC, it seems to vary from different sources from 44C to 68C. Aldrich got values 58-60C and 64-67C

the boiling point of DMT is 160ºC

--

Also this method if it were to work, would likely not be effcient or more pure then a non polar extraction, actually it would be less pure because you would also be distilling oils and other volatiles and constituents of the root bark.


Hum, bad news. You mean 160ºC when the DMT stills inside in the plant, don't you? Because everything I've read about consuming the cristals with a vaporizer or DMT-machine, reports temperatures about 65ºC +/-5ºC

Even more bad is the thing that this method would give the same or more impurities than the common one Sad

geko42 wrote:
swim is curious on why not using a non polar extraction? are you just exploring?


Tell him/her that this is some kind of weird idea from a newbie Laughing

I'm a little bit afraid of chemicals due to possible toxic remains (but not of working with them, I've done it before at the university when I was making lab practices). I was thinking about this because for me, a newbie, sounded like something more pure, simple and safer, and also it would have the clear advantage of obteining the cristals faster than the others.

benzyme wrote:
oh and istubar, that won't work. you're going to have to isolate the alkaloids
before distilling them. don't fear the chems.


Then, which method would you recommend? My priorities are: 1º Healthiest as possible, 2º less time to spend on it. The other things (price, compounds, steps, labware, etc. are secondary)

Maybe it will sound so obvious to more than one, but I'm learning and rediscovering my old chemestry knowledges Confused

Thank you very much one more time!
 
benzyme
#10 Posted : 2/11/2012 4:28:17 AM

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healthiest? brew ayahuaca.
"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
#11 Posted : 2/11/2012 4:36:21 AM

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But I feel that playing with IMAO's it's a little bit risky... besides puke it's not pleasant (specially for your throat due to the acid of the stomach).

Everything you do of course it's healthier if you don't done it Laughing but if you have the requirement of afford some risks, then it's better with minimun ones.
 
۩
#12 Posted : 2/11/2012 4:39:25 AM

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Harmalas are RIMA (reverse inhibitors of monoamine oxidase) and are in no way as risky as true MAOI.
You only really need to watch out for certain pharmaceutical medications like SSRI.
Read more in-depth about this here https://wiki.dmt-nexus.m...edication_interaction.3F
 
benzyme
#13 Posted : 2/11/2012 4:40:27 AM

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well then, I don't know what to tell ya

naphtha is as innocuous as most solvents get, aside from water.
it's not particularly unhealthy.
"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
 
Wonderpus
#14 Posted : 2/11/2012 1:00:20 PM

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If you're really focused on health, you could use pentane or heptane rather than naphtha, which contains n-hexane, an unusually toxic hydrocarbon. With pentane, your extraction will be super quick because DMT precipitates easily from cold pentane, and you'll also end up with a nice pure product. However, pentane won't get all of the DMT, so there's sort a trade-off there. If you use a heavier solvent, say naphtha, you'll get more product, but it'll be less pure and take longer. You can use d-limonene, which is orange oil, all natural, and food grade lye. Now, this might sound appealing, you're thinking "ooh, orange oil, that sounds nicer than those chemicals", but with that stuff, you're pulling all sorts of stuff that the pentane doesn't pull, and you end up with a less pure product. So, what do you see as less healthy? Using pure fractions to get clean crystal, or using natural oil but getting a less pure product and having to smoke some plant fat? If I were you, I'd use pentane first, freeze-precip the pulls, then once your done with that, chuck some limonene or xylene in and pull the "jungle spice". Two grades of DMT, you can decide which you like more!
 
gibran2
#15 Posted : 2/11/2012 1:52:05 PM

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benzyme wrote:
that doesn't sound like dmt. otherwise, how would you be able to vaporize it?
compounds which decompose do not have boiling points. there seems to be a lack of several constants for dmt, but you don't vaporize DMT at 0.8 hPa, do you?

ACD/Labs calculates 332 C at 1 atm

http://www.chemspider.co...ical-Structure.5864.html (properties-->predicted-ACD/Labs)

Hmm... If DMT didn’t decompose, then why would one need to calculate/extrapolate/predict the B.P. at standard pressure, rather than just determine it experimentally?

Have you ever placed DMT in a vial, heated it, and watched it boil?

Also, many substances will give off copious amounts of vapor long before reaching their boiling points. Heat some cooking oil on the stove and you’ll notice it begins to smoke/vaporize long before it boils. (Don’t try this at home, kids!)
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benzyme
#16 Posted : 2/11/2012 1:55:55 PM

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actually, yes I have
on an erlenmeyer flask on a hot plate. the product recrystallized on the sides and on a glass tube as light pink crystals. I didn't measure the temp with an IR thermometer, but I set the plate to 250 C, it usually runs hotter.

Infundibulum brought up an interesting point in one of his posts, one that makes sense, and now that I think about it, may coincide with what you're saying...
the ethyl moeity between the indole and amine have carbons with rotatable bonds; this may attribute to the fact that there is variable melting/boiling points observed, due to intramolecular forces at work. if what you infer is the case, it could be that with enough heat applied quickly, the disubstituted-ethylamine may dissociate from the indole

I've never observed this, dmt has always vaporized (boiled off) then recrystalized when I heat/cool it.I just need to accurately measure the temp as it occurs
"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
#17 Posted : 2/11/2012 4:45:07 PM

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Wonderpus wrote:
If you're really focused on health, you could use pentane or heptane rather than naphtha, which contains n-hexane, an unusually toxic hydrocarbon. With pentane, your extraction will be super quick because DMT precipitates easily from cold pentane, and you'll also end up with a nice pure product. However, pentane won't get all of the DMT, so there's sort a trade-off there. If you use a heavier solvent, say naphtha, you'll get more product, but it'll be less pure and take longer. You can use d-limonene, which is orange oil, all natural, and food grade lye. Now, this might sound appealing, you're thinking "ooh, orange oil, that sounds nicer than those chemicals", but with that stuff, you're pulling all sorts of stuff that the pentane doesn't pull, and you end up with a less pure product. So, what do you see as less healthy? Using pure fractions to get clean crystal, or using natural oil but getting a less pure product and having to smoke some plant fat? If I were you, I'd use pentane first, freeze-precip the pulls, then once your done with that, chuck some limonene or xylene in and pull the "jungle spice". Two grades of DMT, you can decide which you like more!


Hum, that sounds really interesting!

When you said "won't get all the DMT", You mean less mg or less effects? Can I use limonele after using naptha or pentane? Or it only will works with pentane? (because limonele cannot eliminate n-hexane)
 
Istubar
#18 Posted : 2/11/2012 6:58:38 PM

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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?
- In step #1, How many hours do you recommend?
- In step #2, How many ml of pentane? (and how many hours of resting too)
- 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?
- How many hours should the liquid spend in the freezer? Is better freezing than evaporating, isn't it?
- 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?

- Do I forgot something?

Thank you very much for your patience Embarrased
 
Istubar
#19 Posted : 2/12/2012 7:46:58 PM

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Someone can help me a little bit please? Embarrased
 
gibran2
#20 Posted : 2/13/2012 12:20:56 AM

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benzyme wrote:
actually, yes I have
on an erlenmeyer flask on a hot plate. the product recrystallized on the sides and on a glass tube as light pink crystals. I didn't measure the temp with an IR thermometer, but I set the plate to 250 C, it usually runs hotter.

Infundibulum brought up an interesting point in one of his posts, one that makes sense, and now that I think about it, may coincide with what you're saying...
the ethyl moeity between the indole and amine have carbons with rotatable bonds; this may attribute to the fact that there is variable melting/boiling points observed, due to intramolecular forces at work. if what you infer is the case, it could be that with enough heat applied quickly, the disubstituted-ethylamine may dissociate from the indole

I've never observed this, dmt has always vaporized (boiled off) then recrystalized when I heat/cool it.I just need to accurately measure the temp as it occurs

Sorry I didn’t respond sooner, but my internet connection was down for most of the weekend.

The point I was making was that many (most?) liquid substances can vaporize/evaporate well below their boiling points.

For example, heat some water to 200°F, and it will steam, but not boil. Place a fan in font of a shallow pan of acetone or ether and it will evaporate very quickly.

DMT can be “evaporated” at a temperature well below its theoretical standard pressure boiling point.
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