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Several questions about A/B and re-x Options
 
#1 Posted : 10/26/2016 12:42:06 AM

Psilosopher


Posts: 205
Joined: 30-Jul-2012
Last visit: 28-Nov-2022
Location: International waters
Hi everyone!

I've previously used Cyb's Max Ion to do 100g MHRB extractions, which worked great.
However, after a mishap where an evaporation dish wrapped in saran wrap ended up stinking up my whole freezer for weeks on end I now always entirely evap instead of freeze precipitate.

I have far less free time on my hands to do extractions these days, and I still have quite a bit of bark sitting around that I'd like to extract as soon as possible.
In the past week, I've done 5x 2 hour long acid boils at pH 3 on 500g MHRB, and combined the resulting liquids in glass carboys.
My idea is to simply reduce this liquid (now around 5 liters) to a manageable level and then basify and extract it. However, I still have a few questions I'd like to resolve before I proceed further.

My previous extractions I ended up with quite yellow DMT. I didn't have the best extraction tools available to me at the time, and so a few things happened which I guess could have caused my less than optimal results:
1) I let the basified goop sit for up to a month, doing just one pull every weekend. Often I could also not entirely separate the naphtha and a tiny layer of naphtha remained in there all that time, likely absorbing undesirables
2) I didn't have the best pipette and ended up with some bark/lye in my evaporation dish. I figured no problem as I was going to re-x it anyway.
3) My naphtha was yellow when I did the pulls, I found several topics on this and several people seem to suggest that when starting with powdered MHRB (I did) these fine particles can get suspended in the naphtha when agitating. I also have seen people saying that they were "unable to clean it up however they tried, only a mini-A/B helped". I might try that in the near future.

I did 3 re-x's, and while the DMT went from brownish goo to a more or less freeflowing dark yellow powder, I didn't end up with the white crystals I was imagining (again, I didn't freeze precipitate, just re-x and evap). I've smoked the yellow powder I ended up with, but 15-20mg smoked in the GVG gave me only slightly above threshold effects: a pleasant heavy body high and slight visuals, far less intense than say 100ug LSD. The rapid shift in consciousness was definitely there and at times very startling, but it has given me only pleasant light experiences, nothing profound.
I'm fairly sure I vaporized it correctly as the vapor was smooth and pleasant by all means.
So I'm assuming I still have a bunch of impurities in there that I somehow can't seem to be able to clean up, and this is why I can't seem to get off on what should be decent dosages.
I thought that maybe I had DMT-oxide since my bark was also quite old, but I've since read that DMT-oxide is not soluble in naphtha/heptane, so I guess that rules it out..
Here is what it looks like:



Now, I would like to do everything possible to end up with a better quality end result with this new extraction, of course. Here is what I'm wondering:

1) When reducing my acid boils, is there a minimum amount of liquid I shouldn't go below? I assume 500ml would be a decent amount, but would it for instance be possible to reduce it to only 250ml or so? I'd assume the lower the total volume, the more concentrated the dmt and the easier it will be to mix the naphtha in as the ratio liquid/naphtha will be lower and it will be easier for the solvent to fully contact all of the liquid without having to excessively shake it.

2) Can I reduce with a good rolling boil on high heat, or is there any danger of evaporating/destroying the dmt in the process? I've looked this up, and people seem to agree that DMT can be boiled very vigorously without issue (as is often done with brewing aya). I would obviously stir it constantly, and reduce heat once the volume drops considerably.

3) If particles of powdered MHRB could become suspended in naphtha, would it be better to filter my liquid a bunch of times to get as many of these particles out as possible? I don't have great equipment for this, only a funnel with a mesh screen and a cheesecloth, but maybe it's worth trying to filter it a bit beforehand for a cleaner product?

4) Should I heat my basified solution for a few hours and let it cool back down to room temp, or can this step be skipped? I've read that when doing this you are more likely to pull more impurities? Though I assume the heating helps free up the DMT in the solution as well?

5) I've always used (near-)boiling naphtha to do my pulls. Maybe this also caused me to pull a lot more impurities and I should switch to using just "warm" solvent instead?

One more question about recrystallization that I've asked in a number of places/forums, but never got a clear answer on:
I add some heptane to impure DMT and slowly heat it up. How do you know when all/most of the DMT has migrated into the warm heptane and only impurities are left behind? I usually heat my heptane up quite hot, and then just a little bit of sediment remains. Maybe I'm heating it up too much and impurities start to dissolve into the heptane as well, still leaving me with an impure end result?
Where exactly do you draw the line how much heat is perfect when recrystallizing?


Sorry for this long post, I just wanted to get everything straight before I proceed so that I can improve my extractions.
"The only way to deal with an unfree world is to become so absolutely free that your very existence is an act of rebellion." - Albert Camus
 

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fathomlessness
#2 Posted : 10/28/2016 12:47:39 PM

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ॐ wrote:


1) When reducing my acid boils, is there a minimum amount of liquid I shouldn't go below? I assume 500ml would be a decent amount, but would it for instance be possible to reduce it to only 250ml or so? I'd assume the lower the total volume, the more concentrated the dmt and the easier it will be to mix the naphtha in as the ratio liquid/naphtha will be lower and it will be easier for the solvent to fully contact all of the liquid without having to excessively shake it.


On multiple cooks I have had problems with basified emulsions if I go below 1/4 of the original volume before i basify but I only filter through a t-shirt in the acid stage.
ॐ wrote:


2) Can I reduce with a good rolling boil on high heat, or is there any danger of evaporating/destroying the dmt in the process? I've looked this up, and people seem to agree that DMT can be boiled very vigorously without issue (as is often done with brewing aya). I would obviously stir it constantly, and reduce heat once the volume drops considerably.

Dmt-acetate and DMT-hcl are both very stable at high temps. I have reduced at high boiling temps before and never reported loss and I have never heard anyone reported loss. I use high boil and in the open air for faster evap. Once it gets to a certain volume it no longer boils but froths until it overflows from the pot. it has happened a few times and made me Mad

Quote:
3) If particles of powdered MHRB could become suspended in naphtha, would it be better to filter my liquid a bunch of times to get as many of these particles out as possible? I don't have great equipment for this, only a funnel with a mesh screen and a cheesecloth, but maybe it's worth trying to filter it a bit beforehand for a cleaner product?


Naphtha contam is rare but I have had it a few times. You have to remember that some naphtha will be lost in the filtering mechanism be it cheesecloth or coffee filter. I let the naphtha sit for a few hours at room temp and let the particles fall to the bottom then pour off in to new container.

Quote:
4) Should I heat my basified solution for a few hours and let it cool back down to room temp, or can this step be skipped? I've read that when doing this you are more likely to pull more impurities? Though I assume the heating helps free up the DMT in the solution as well?

Heat to what temp? Don't go higher than 50c. really you only need room temp or 30c. If you are trying to reduce emulsions then use more water or more lye, or don't shake so hard.

Quote:
5) I've always used (near-)boiling naphtha to do my pulls. Maybe this also caused me to pull a lot more impurities and I should switch to using just "warm" solvent instead?


if dmt goes in to boiling naphtha then dmt is going to be kaput when it goes in isnt it? Warm is safer.

Quote:
One more question about recrystallization that I've asked in a number of places/forums, but never got a clear answer on:
I add some heptane to impure DMT and slowly heat it up. How do you know when all/most of the DMT has migrated into the warm heptane and only impurities are left behind? I usually heat my heptane up quite hot, and then just a little bit of sediment remains. Maybe I'm heating it up too much and impurities start to dissolve into the heptane as well, still leaving me with an impure end result?
Where exactly do you draw the line how much heat is perfect when recrystallizing?


I use naphtha to re-x and do a warm water bath so the naptha gets around 30-40c and then use my finger to rub it in for about a minute. What remains is a lot of goo at the bottom, this goo is still DMT in its goo form, as DMT is polymorphous (has two states a crystal and a goo). So instead now I convert to fumarate and then base again. OR freeze the naphtha and then just dry the goo and make some changa with it.
[/quote]
 
Tryptallmine
#3 Posted : 11/5/2016 8:45:10 PM

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fathomlessness wrote:
[quote=ॐ]

Quote:
5) I've always used (near-)boiling naphtha to do my pulls. Maybe this also caused me to pull a lot more impurities and I should switch to using just "warm" solvent instead?


if dmt goes in to boiling naphtha then dmt is going to be kaput when it goes in isnt it? Warm is safer.



By kaput do you mean lost or damaged?

Boiling naphtha won't hurt DMT as this is what we do in a Re-X. I've never gotten my head around the boiling naphtha thing. The temperature equalization would happen so rapidly (50ml NPS on 2Lt Aqueous) that it wouldn't justify warming it up above that of your aqueous phase (~50c). I stopped warming it up altogether and simply poor it at room temp out of a beaker.

DMT solubility increases as solvent temperature increases - which is the theory behind why people want to boil it for pulls.

The reasons that stand out to me that your spice turned yellow are that you boiled it and left it sitting for a month. Anytime I've used high heat or boiled an acid phase I end up with incredibly colorful/yellow DMT. You just pull more pigmentation than you would if you heat bath it @ 45-55c. Additional leaving based aqueous sitting for weeks also decomposes more plant material and adds to the pigmentation.

If you want to check for contamination, re-x it, however there's nothing wrong with yellow spice! Yours looks delicious..





 
#4 Posted : 11/6/2016 4:08:20 PM

Psilosopher


Posts: 205
Joined: 30-Jul-2012
Last visit: 28-Nov-2022
Location: International waters
Thanks for the replies!
I already reduced my 5 acid boils down to around 500ml, I'm going to be extracting it in a few days, not really going to follow a particular tek but simply basifying it to pH 12-13 and pulling with hot heptane, standard A/B.
I'm curious what the yield will be and if it will come out more white than last time.
I saved my boiled bark in case there's some dmt left in there.

As has been pointed out, I use (near-) boiling solvent to do my pulls since I've read this increases dmt's solubility in it. I know the temperature reaches an equilibrium just seconds after throwing it in, but I figure it still might improve the amount per pull if just a little bit. Would also like to point out I'm heating the solvent in a glass erlenmeyer on a sparkless hotplate, if I didn't have that I wouldn't risk heating it up too much..

fathomlessness wrote:
Quote:
4) Should I heat my basified solution for a few hours and let it cool back down to room temp, or can this step be skipped? I've read that when doing this you are more likely to pull more impurities? Though I assume the heating helps free up the DMT in the solution as well?

Heat to what temp? Don't go higher than 50c. really you only need room temp or 30c. If you are trying to reduce emulsions then use more water or more lye, or don't shake so hard.


First time around I used Cyb's Max Ion, which specifies the following for the basification step:

Quote:
4. Dissolve apprx 40g of NaOH (Lye) in a minimal
amount of COOL filtered water (approx 100ml) and
add to the acidic/saline mix.
A pH of 12+ is desired, so add more if necessary.
5. Warm the mix in the heat bath for 2 hours
(stir occasionally)
{Low heat, the glass vessel should be able to be
handled without burning}
6. After 2 hours, cool to room temperature.


I'm not 100% sure what the heating is supposed to do, I assume it helps the breaking down of the bark along with the base? Maybe heating the solution up isn't really necessary when pulling from a filtered acid boil solution instead of from a mixture that still has all of the bark in it?
"The only way to deal with an unfree world is to become so absolutely free that your very existence is an act of rebellion." - Albert Camus
 
#5 Posted : 11/18/2016 11:37:11 AM

Psilosopher


Posts: 205
Joined: 30-Jul-2012
Last visit: 28-Nov-2022
Location: International waters
Thought I'd post a quick update:
The first two pulls of my recent extraction are done, and I couldn't be more happy with the results, I have yet to weigh it all out, but I ended up with a pile of much purer crystals this time around. The majority of the xtals are pure white, some have some slight pale yellowing, but all in all it looks much, much better than what I got last time (in the picture of my OP).

My conclusions:
- Don't let the basified bark sit for weeks on end, do the pulls shortly after basifying
- Don't use excessive heat (in fact, this time I didn't heat up the bark mixture at all, just basify, cool off and pull)
"The only way to deal with an unfree world is to become so absolutely free that your very existence is an act of rebellion." - Albert Camus
 
 
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