CHATPRIVACYDONATELOGINREGISTER
DMT-Nexus
FAQWIKIHEALTH & SAFETYARTATTITUDEACTIVE TOPICS
Distilling off excess solvent before freeze precipitation instead of open air evaporation Options
 
Dimethylentity
#1 Posted : 10/1/2018 7:23:23 AM

I am an autism and love to role play as a fractal embroided insectoid stick figure looking shadow that seamlessly projects itself between dimensions... So don't take anything i say to be real by any means.

New member

Posts: 9
Joined: 12-Aug-2018
Last visit: 18-Nov-2018
Location: Here?
Alloo!
Was wondering if anyone has tried this or does it to reclaim their solvents. Couldn't find any thread relating to it.

Got some 99%+ ACS heptane for the initial pulls and want to maximize it's re-usability as it was not cheap..
I understand that a naphtha blend would be better for the initial pulls but it is hard to find clean naphtha where i am and i don't want to order it online.

So what my idea is, once the the nps has been pulled from the base soup, instead of evaporating (into open air) down to the point of saturation before freeze precipitation i want to do the exact same thing but in a distillation rig so the "clean" solvent can be collected for reuse.

Would this be a viable rout to recover solvents for reuse? Or would this cause excessive oxidation of the dmt from being heated for the period of time it takes to distill the solvent down?

Using heptane instead of naphtha, am i right in thinking that the oxidation rate would be increased due to the higher boiling point of heptane?

Very interested to hear any experiences or any expertise in the matter Smile

Lot's of love!!! Big grin
 

Psychedelic news, articles, interviews and art from the DMT-Nexus and other sources.
 
pete666
#2 Posted : 10/1/2018 7:50:29 AM

DMT-Nexus member


Posts: 499
Joined: 13-Jan-2018
Last visit: 15-Dec-2018
I don't have experience with such distillation, but just for your information, there is another alternative to this, not requiring any excessive heating. You can titrate/back-salt the alkaloids from the non-polar solvent. Non-polar can be immediately used for next pull. Then basify acidic solution by NaOH and extract/re-x by hot heptane. No need to evaporate non-polar this way at all. I suggest doing titration, not just back-salting, as knowledge of alkaloid content is convenient for subsequent heptane pulling.
Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
downwardsfromzero
#3 Posted : 10/1/2018 5:13:34 PM

Eggnogstic - warning! Self-irony levels: high!

Chemical expertSenior Member

Posts: 3511
Joined: 30-Aug-2008
Last visit: 14-Dec-2018
Location: square root of minus one
Regarding the boiling temperature, while heptane boils at 98°C, the boiling range of naphtha depends entirely on the exact blend of components. Thus naphtha could boil at a high or lower temperature than heptane depending whether it's a light, medium, or heavy naphtha.

If you were worried about oxidation of product when distilling, an inert atmosphere such as nitrogen or argon would protect things. If it's thermal decomposition that concerns you, vacuum distillation would help circumvent this.

One potential problem with distillation is entrainment of the DMT freebase, so it co-distils with the solvent. This I have seen occur with heavy naphtha, b.p. ca. 130°C. That makes the solvent reduction distillation process somewhat pointless in such an instance - unless there are non-volatile components you wish to distil away from.

Distillation also requires more complicated equipment, and a higher level of expertise considering the additional dangers of heating a flammable liquid.

All that said, there shouldn't be too much co-distillation with heptane - but only practical experimentation would allow us to be sure one way or the other. Thus I would go along with pete666's suggestion, unless I really wanted to test the co-distilling question w.r.t. heptane.


(I heartily approve that you're thinking along these lines and not simply evaporating your solvent Thumbs up )
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
Dimethylentity
#4 Posted : 10/8/2018 9:21:01 AM

I am an autism and love to role play as a fractal embroided insectoid stick figure looking shadow that seamlessly projects itself between dimensions... So don't take anything i say to be real by any means.

New member

Posts: 9
Joined: 12-Aug-2018
Last visit: 18-Nov-2018
Location: Here?
pete666
Hmmm.... I just feel silly now for even thinking of bringing heat into the equation! Laughing
Back salting hadn't even crossed my mind.. lol
Haha i feel like my approach was like "Using some enormous instrumentality to solve a trivial thing" - Terence Mckenna

Ok so using back salting or titration to to get the goods out of the bulk of solvent, rebasing and then use a minimal amount of solvent to recollect for freeze precip.
The reasoning behind using distillation was to completely separate the solvent from almost everything. I'm guessing even back salting there would still be a little something left in the solvent that would slowly build up over many re-uses but i guess if the backsalt trick is done and then you distill the solvent there would be no worry of wrecking anything that was stuck in it, which i'm guessing would be some oils and plant fats.



downwardsfromzero
Yea, been very interested in these inert atmospheres but confidence seems to dwindle away at that level of coggigerymerbobbing with this stuff Confused
Just jerry rigged a vacuum filter last night with a glass funnel and jar lid lol Sorta works when it wants to.
Vac distillation is definitely going on the list on the list! No jerry rigging for that, for safety.

Successfully (no kaboom) distilled some dirty tech grade solvent before, though there was no internal thermometer so it was kind of a blind experiment, a bit of residue ended up in the distillate but not sure if that was from over boiling or something that was already in the glass wear. Used vegetable glycerine to seal the joins so a bit may have seeped in..
It boiled 3-4 fraction between 30C-75C.

Ohhh riight, hadn't though of co-distillation.. That could be fiddly to deal with, even with fractional distillation.
Do ya reckon most of of the co-distillate would get caught in the fraction column and re-solidify there?

Guess the only way to know is to give it a whirl and try it...
Got a wee list of 'Why would you do that when you could do this' techniques like this that shall be put to the test sometime Smile

If it works will post results here.
 
pete666
#5 Posted : 10/8/2018 11:21:35 AM

DMT-Nexus member


Posts: 499
Joined: 13-Jan-2018
Last visit: 15-Dec-2018
Dimethylentity wrote:
pete666
Ok so using back salting or titration to to get the goods out of the bulk of solvent, rebasing and then use a minimal amount of solvent to recollect for freeze precip.
The reasoning behind using distillation was to completely separate the solvent from almost everything. I'm guessing even back salting there would still be a little something left in the solvent that would slowly build up over many re-uses but i guess if the backsalt trick is done and then you distill the solvent there would be no worry of wrecking anything that was stuck in it, which i'm guessing would be some oils and plant fats.


I am sometimes reusing the same solvent even without cleaning. I don't have problem to re-x at the end though if I am not happy with the result. The solvent can be cleaned up of course. Check here.
Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
blue.magic
#6 Posted : 10/8/2018 5:28:43 PM

DMT-Nexus member


Posts: 931
Joined: 11-Feb-2017
Last visit: 12-Dec-2018
Yes! This is exactly what I do now.

Both simple distillation setup and rotary evaporator work great for this purpose, though rotavap is superior (better heat control and less prone to bumping under vacuum).

I tried naphtha and heptane, but heptane works better as it has a single boiling point. With naphtha, you have to gradually increase temperature to compensate for the sliding boiling point (if you pull vacuum, it is really easy to overheat naphtha - I once managed to siphon it all the way from distillation flask to the receiver Very happy ).

Vacuum helps a lot since boiling point of some naphthas is so close to vaporization temperature of DMT. Yet another reason to use heptane or other solvent.

What I do now is basically the typical lab practice: extract in a solvent, dry the solvent (with e.g. calcium chloride), filter, concentrate in rotavap and finally crystallize from the conc. solution.

Usually less than 5% of the solvent is consumed in each extraction, so one bottle of solvent can be used many times over.

Of course, if you plan to use the distilled solvent for other purposes, it needs to be thoroughly purified and dried. I have lately purified my DCM and even though it looked crystal clear, it was full of organic chemicals, actually pretty dirty.
 
Dimethylentity
#7 Posted : 10/12/2018 4:06:23 PM

I am an autism and love to role play as a fractal embroided insectoid stick figure looking shadow that seamlessly projects itself between dimensions... So don't take anything i say to be real by any means.

New member

Posts: 9
Joined: 12-Aug-2018
Last visit: 18-Nov-2018
Location: Here?
Awesome to hear someones tried it and it works!
So is their any noticeable loss of yield, degrading or oxidizing?
Any tips/tricks for heat and time in relation to those possible issues?

blue.magic wrote:
Vacuum helps a lot since boiling point of some naphthas is so close to vaporization temperature of DMT. Yet another reason to use heptane or other solvent.

Would the vacuum not also lower the boiling point of the desirables as well as the solvent, thus retaining the temperature difference? Or is there something tricky going on there? Razz
Also what downwardsfromzero was talking about (co-distillation), did that present many if any problems at all with solvents with boiling points of 98C or lower?

Smile
 
downwardsfromzero
#8 Posted : 10/12/2018 8:25:53 PM

Eggnogstic - warning! Self-irony levels: high!

Chemical expertSenior Member

Posts: 3511
Joined: 30-Aug-2008
Last visit: 14-Dec-2018
Location: square root of minus one
Quote:
Also what downwardsfromzero was talking about (co-distillation), did that present many if any problems at all with solvents with boiling points of 98C or lower?

I said all that I need to say in my previous post already. Except, inert atmospheres aren't that difficult to rig up. Think welding, or sodastream.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
 
Users browsing this forum
Guest

DMT-Nexus theme created by The Traveler
This page was generated in 0.028 seconds.