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Distilling off excess solvent before freeze precipitation instead of open air evaporation Options
 
Dimethylentity
#1 Posted : 10/1/2018 7:23:23 AM

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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
 

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pete666
#2 Posted : 10/1/2018 7:50:29 AM

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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.
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downwardsfromzero
#3 Posted : 10/1/2018 5:13:34 PM

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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 )




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Dimethylentity
#4 Posted : 10/8/2018 9:21:01 AM

I am an artism 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.


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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

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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.
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blue.magic
#6 Posted : 10/8/2018 5:28:43 PM

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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 artism 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.


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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

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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.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
Dimethylentity
#9 Posted : 8/17/2019 8:00:46 AM

I am an artism 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.


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Hey guys!
Ok so I've been tinkering Smile
I wanted to see if pure dmt freebase would change at all under different high-ish temperature conditions. Mainly the temperature of the highest b.p. solvent I use and distill with the alkaloids still in it (heptane).

Here's the log:
-103mg (+/- 5mg) of white/clear glass shard-like crystals
-Dissolved in 50ml heptane at 40-45C
-When taken off heat the solution clouded at 25-30C and some oily layer settled out in the flask. I'd guess 10-15mg of oil.
-Distilled (simple distilation) off roughly 40-45ml of the heptane, the hotplate was running at 200-222C, 2-3 drops a second. The distillation took about 30 minutes.
-Evaporated the remaining heptane with a cold fan. Almost all the crystals had already precipitated at room temperature before evaporation.
-The crystals looked exactly the same as they did at the start.

So no noticeable thermal degradation has occurred.
So at the very least small amounts of solvent that boil under 100C are safe to run in a simple distillation to get a consentrated solution. It may be different for larger amounts of solvent since the solution will be exposed to the heat for far longer.

Also, i wanted to see if dmt would slowly evaporate or degrade at high-ish dry heat.
Put 15mg-ish of white crystals on some glass on a hotplate and left it at 100C for quite a few hours. The puddle of dmt had no size or color difference and recrystalized to a crumblable wax.
Didn't weight it in the end...

I know that blue.magic already said they concentrate their pulls via distillation but this was a fun experiment and by using very pure dmt it made it very observably definitative.
I would vape it to see if it is the same as before the distillation but this was extracted from bark that had developed mold, it was only a fine white powder looking film on some of the bark but I'm not to keen to risk it. Endlessness said in a thread that he mass speced some extract from moldy bark and no mold related stuff was present but just to be safe I'd rather not. I might have access to a mass spectrometer soon so I may be able to find out.

One other thing, I'm still on that same 2L bottle of heptane Smile
Been doing pulls, freeze precipitating and reusing the yellow heptane and when done with the extraction, distilling off the heptane and making changa with the leftover goo. Recovering roughly 70% of the solvent this way, some does evaporate through out the extraction process but hey, still pretty good!

Peace Smile


First picture is before and the second is after distillation.
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blue.magic
#10 Posted : 8/18/2019 3:53:03 PM

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Yes I do this using vacuum distillation with rotary evaporator and hot water bath.

I pull vacuum to boil heptane at ~50 °C and continue distillation until the solvent is cloudy. Here I think vacuum is beneficial to reduce oxidation/decomposition and you end up with just the right amount of solvent (as it gets cloudy sooner than in hot boiling solvent); but you can as well distill off almost everything w/o vacuum and then top up with some solvent, just to create space for the oils to dissolve.

Then I stop the rotavapping, release vacuum, set water bath temperature to ~70 °C and wait until the solvent gets clear again.

I usually get a small pond of oil on bottom so I decant solvent into dish without the oil, pour fresh solvent into the flask, re-heat in water bath and decant again. I repeat this several times.

Then I proceed with freeze precipitation.

When I do heptane pulls at mother liquor temperature of 40 °C, only one recrystallization is needed to get rid of virtually all the oils.

This extraction method has big advantage of saving solvent and you can use excess solvent.

---

One final thing I do now after freeze precip is to pour solvent from the dish through a filter (vacuum filtration), then quickly scrape crystals and place on filter. The crystals will dry quicker with the vacuum on.

Finally, I wash the crystals with cold heptane, let them dry a bit and then wash with cold 3% ammonia.

The crystals are then dried under vacuum.
 
artificer
#11 Posted : 1/14/2023 1:24:42 AM

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downwardsfromzero wrote:
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 )


Bumping an old thread here, but if I were to make a new thread it would be entirely about ^this^ subject. I did not realize the potential for co-distillation as described above. Any new insight on this since 2019?

I just boiled 750mL n-heptane (pulls from A/B) through distillation apparatus down to 100mL that almost immediately started to form crystals as it cooled to RT (will go to freezer). I did this with some vacuum and n-heptane @ 80°C - have tests been done to confirm lack of co-distillation with n-heptane? Unfortunately I already poured distilled liquid back into heptane bottle.

I also did more pulls with xylene (B.P.≈140°C) and started distillation with it as I came across this thread... is it likely that there's DMT co-distilling with the xylene? If so, would it only be a portion of the DMT? The liquid collecting in receiving flask is crystal clear, while xylene pulls in boiling flask has hazy yellow tinge. If a high enough percentage of DMT is co-distilling, could it actually be taken advantage of, getting a cleaner product doing FASA on the distilled xylene with less demand to do a wash?
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downwardsfromzero
#12 Posted : 1/14/2023 2:46:37 AM

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Quick answer without digging around too much is that member 1ce did a few tests with cyclohexanol as the entrainer back in about 2015. Entrainment depends not only on relative boiling points but on some additional physical properties. In this case an important consideration is the vapour pressure of DMT at the boiling point of the solvent. Intermolecular forces between the solvent and the DMT may also play a role but I'll admit that my knowledge on these details is a little patchy.

I would not be at all surprised if you found that a detectable if not significant amount of DMT co-distilled with xylene. Vacuum distillation might change this but you'd best see if there's a vapour pressure/temperature chart for DMT somewhere if you want to make plans to try stripping only xylene off.

Definitely seems worth testing a portion of your distillate with FASA and maybe to proceed with the rest of it if it seems like a decent amount of fumarate crashes.

The yellow colour suggests some polymer/oligomer gets left behind. Maybe this can be recovered with a backsalt/mini A/B?




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
artificer
#13 Posted : 1/14/2023 8:31:00 PM

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I appreciate quick reply DF0 - know that it's not taken for grantedWink

I've yet to do backsalting/mini A/B on anything yet, I've seen it mentioned all over the place here, but not a specific "backsalting tek" - how I understand it, I should mix xylene pulls with an acidic solution, shake it all up well, let separate, and collect the aqueous solution to basify and pull with NPS. Any pointers here? Is vinegar, HCl, or citric acid preferred for acidic solution? After basifying, the go-to would be naptha for some jungle spice or heptane for pure DMT, correct?

Since freebase is my ultimate goal with this batch, I'll probably try backsalting both the distilled and yellow xylene, separately, to see how much got co-distilled.
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downwardsfromzero
#14 Posted : 1/15/2023 10:19:42 PM

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Since you can use FASA with xylene it might seem to make sense to do that on both portions if you've lined it up already. I am wondering how fumaric acid behaves alongside oligomerised DMT however - whether it can polymerise in practice as it would appear to be able to do in theory is not something I can predict. i can envisage a small possibilty that the unpaired electrons involved with DMT oligomerisation might act as free-radical polymerisation initiators for an unsaturated acid like fumaric, or maybe they could cause isomerisation to maleic acid.

It's a bit late in the evening and I've been entertaining a guest so I'll have to reserve further speculation for now. My fumarate didn't behave itself when I took my time over it (surprise, surprise!) some time ago so it feels like these ideas may have some level of merit.

Maybe mini A/B is the way to go. Vinegar is as good as anything, I'd say. Citric acid is a more complicated molecule. Your understanding of the process appears to be correct.




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
artificer
#15 Posted : 1/24/2023 6:18:06 PM

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Just a quick follow-up here - I started with approximately 750mL xylene (from A/B pulls), distilled it down to about 100mL and captured the 650mL that evaporated. This was done with distillation apparatus and roughly 850 millibar vacuum (≈.84 atmosphere). Temperature reading of the boiling liquid was 120°C and vapor 80-90°C. I back-salted and performed mini A/B to both the 100mL and the 650mL separately. Yield from the 100mL concentrate was 1.4 grams DMT (freeze precipitated 180mL naphtha @-20°C); yield from the 650mL distilled xylene was 0grams (freeze precipitated 95mL naphtha @-20°C), so no measurable co-distillation took place. Of course results may have been different with no vacuum and higher temperature boil during distillation.
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downwardsfromzero
#16 Posted : 1/24/2023 7:53:37 PM

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Excellent - thanks for sharing the results! Any kind of data, even a negative result, is of value to the communityThumbs up




“There is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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