Freez precip stage gone wrong

[stationdragon]

I've recently tried my hand at a few extractions using MHRB and following Nomans tek but with the addition of salt at the lye/water stage to help force more DMT into the naphtha.
The previous few have gone very well and I've been more than pleased with the results, but this last one has gone wrong and I don't know why.
My process is to powder the bark, add 1ml water per gram of bark, 1g of lye per gram of bark and 1g of salt (without additives or anti-caking agent) per gram of bark into a HDPE plastic container along with the bark and shake it up. Leave for one hour and then add the naphtha (1ml per gram of bark), I roll it around slowly and rest, repeat 3 more times and siphon off the naphtha. I then repeat this process 4 times and collect the naphtha in jars before freezing them at a very cold temperature.
Within a few hours the crystals have precipitated out and collected on the sides and bottom of the jar.
This time though there are no crystals forming, just a white slime/stringy film. Has anybody got any clue as to what has happened here or if there is anything that can be done to save it?
I changed nothing in the process, nothing at all. The only thing different was I opened a new container of lye, but I don't see what could have caused this.
I look forward to your ideas.

Thanks

 

[steppa]

I ran into the same problem multiple times. If it happens it happens mostly after the third or fourth pull.
While beeing in the freezer it goes to a jelly fish like consistency. The only thing that helped me in These cases was to take it out of the freezer, warm up the whole thing so that everything goes back into the solution, add more naphta and put it in the frezer again.
I guess that adding more naphta reduces the concentration of the stuff that leads to the jelly fish phenomena.

Actually I'm having a case of jelly fish right now! But this time it occured while rextalizing with heptane.

Any thoughts on this?

How to avoid the jelly fish phenomena?
What exactly causes the jelly fish phenomena?
How to neutralize it if it occures?

 

[stationdragon]

Thanks for sharing, it's good to know I'm not the only one.
This has happened to all of my pulls which is odd as yours only happens from the third. The only thing I can think of is I let my friend wash the jars last time and I wasn't there to monitor him so there may be a chance he washed them with the rest of the dishes and perhaps there was some sort of residue left behind. I can test this theory because the final jar I washed as it was being used for something else at the time and I know it's clean. One more pull and some freezer time and I'll know.
Other than that I'm going to warm the naphtha as you suggested, add more and I will add it back to the lye/MHRB solution in the hope that any residue that may be left in the jar will sink into the dark layer.
I will update on this as I get results.
Thanks again

 

[steppa]

and I will add it back to the lye/MHRB solution in the hope that any residue that may be left in the jar will sink into the dark layer.
I will update on this as I get results.

Good Idea. Let us know how it worked.

I'm still unsure how to deal with my heptane jelly fish. :|

 

[ZenSpice]

Is the heptane heated up prior to re-x?

From my own re-xing I noticed that if heating the heptane (carefully with a heated water bath technique) that the solution will crash out as it cools, starting to cloud and create formations before any real evap phase has chance to start..

I think (from my own observations) that as it cools, it forms layers. The lower layers that crash out first contain additional "gunk" (bad term but am sure you get me) and the top layers are cleaner. I don't think it's "jungle spice" as I believe you can't get this from Mimosa. Possibly some plant oils/fats carried along in the solvent (wiser people on here will know).

After a few experiments with re-x I managed to separate the two, ending up with a large amount of white crystals and a small amount of slightly yellowish wax.

Am still learning myself but that's my humble bit of input.

 

[alert]

don't think it's "jungle spice" as I believe you can't get this from Mimosa.

Mimosa is the source plant where the term "jungle spice" originated. Whether you pick any up or not is dependent on what solvent you are using.

 

[steppa]

Am still learning myself but that's my humble bit of input.

Thank you for this!

Is the heptane heated up prior to re-x?

Yes. I heated the heptane in a water bath (pretty hot). Put the reddish/brownish spice from my last naphta pull in, stirred, waited 5 to 10 minutes to let it settle and then decanted into the precip dish.

I think (from my own observations) that as it cools, it forms layers. The lower layers that crash out first contain additional "gunk" (bad term but am sure you get me) and the top layers are cleaner. I don't think it's "jungle spice" as I believe you can't get this from Mimosa. Possibly some plant oils/fats carried along in the solvent (wiser people on here will know).

After a few experiments with re-x I managed to separate the two, ending up with a large amount of white crystals and a small amount of slightly yellowish wax.

I not really sure but I think might be right about the layers. I think I'll try the following:

I'll heat it all again so that all the gunk and xtals go back in the solution. Then, when it cools down again I'll have an eye on it. What I'm hoping for is, that the gunk chrashes out earlier than the xtals. If so I'll just strain it through a coffee filter, pre wetted in heptane so that it doesnt suck up so much of the spice saturated heptane.

Thanks for your input. Will report how it went.

The bummer is that I got the hepane because I thought it lead to better results when reXing. Funny how things go sometimes...

 

[ZenSpice]

Alert thanks for the correction.. A dumb momentary mix-up moment from myself.. I think I was wrongly recalling a convo about the chances of Yuremamine which was, as you say, dependent on the NPS used.

So yeah, the selectivity of solvents I use I believe are the reason I don't get jungle spice (from what I gather again I am happy to be corrected if wrong as defo in learning stage myself). I've used LPD and Heptane, not had chance to try Limonene and the like. I mention as I recall talk of Limonene and from recollection think this is kind of solvent people have used to pull more alkaloids (and plant fats/oils) out.

On the heptane tip, I am sure I recall reading something about a layer change at (roughly) the 40 degree mark..

As is, this is just me "vibing" back and forth hoping to learn, work out if I have things right in my head and to stand gladly corrected if need be (best way to learn imo). :thumb_up:

Thanks

 

[stationdragon]

I decided to try steppa's advice to redissolve the strange precipitate and add more naphtha before putting it back in the freezer. I also decided to hold off my idea of adding the naphtha back into the black solution until ~I had tried this because if steppa was right about the solvent being too heavy with DMT and therefore causing the "jellyfish" effect, then I was concerned that putting it back into the mix might make it pick up further DMT and lead to the same effect, and as I'm low on naphtha I can't add much more to compensate.
Anyway I tried the original idea presented by steppa and it hasn't worked for me, they've been in the freezer for a few hours now and I've just had a peek to find the same milky/stringy solution.
My next step will be to trying adding it to the solution in the hopes that any junk will sink out of it.
Updates to follow.

P.s. thanks for all the interest in this subject

 

[ZenSpice]

Just a laymans thought but did you evap any of the solvent off prior to freeze precip?

This might help to get a better result, or something a bit more workable for re-x.

Also give it a good 12+ hours in the freezer (I aim for 18). If it is a later set of pulls then 24+ after a good partial evap. Apologies if this is going over things you have done anyways.

 

[steppa]

~I had tried this because if steppa was right about the solvent being too heavy with DMT and therefore causing the "jellyfish" effect

I sure that the jellyfish effect is not caused by too much DMT in the solution, you got me wrong on this. But I think it's caused by some stuff that gets pulled along with the DMT.

Sad to hear that it didn't work out for you. It worked for me at least twice. Hope that you get it right soon. If so, please tell us how.

 

[DreaMTripper]

Its the alkaloids in suspension half way between being dissolved and precipitated , , like hyperlimbo! It hangs waiting to breakthrough but just slides away I saw someone extract with sunflower oil and it just imprisoned the dmt in impenetrable heavy oil but it extracted it in seconds!
If you put the np in first after heating it bubbles up catching the alks in one swoop like some sort of whitches brew

 

[steppa]

If you put the np in first after heating it bubbles up catching the alks in one swoop like some sort of whitches brew

Would you mind clarifying this a bit? It sounds like it could be useful knowledge, but I didn't really understand how it's meant. Heating what? The np solvent or the whole mix? In my last pull I used hot naphta, while my mix was at room temp.

 

[stationdragon]

Hi, well my latest effort has ended with the same result but less intense.
I redissolved the DMT and stringy substance by heating the solvent a little and swirling around. Let it cool to room temperature and added it back to the solution and siphoned off, jar by jar (washing the jars thoroughly in between).
The solvent went in with a yellow tinge and came back very yellow.
DMT crystals formed on the pipette in between uses too.
The jars went back to the freezer and after several hours I've looked at them to find the same substance but less of it, with waxy DMT stuck on the bottom.
I did not evaporate before putting in the freezer but I heard this can cause the jelly to form anyway. I'm confused though, on one hand I'm being told to add more solvent and on the other I'm being told to evaporate some. Out of curiosity what do you think would happen in each instance and what is your reasoning behind it?
I too would like clarification on DreaMTripper's advice, I was a little confused by this too.
Does anybody know of a surefire way of fixing this current extraction? Also what would cause this if I did everything exactly the same as before, measurements, time scale, everything?

Thanks for your continued help.

 

[DreaMTripper]

Heat the NP then pour into an empty jar. Swiftly but steadily and carefully add the basified bark/phyllode soup ontop of warm/hot NP in this new jar so it rises through the soup collecting the alkaloids on the way.

 

[whitebread420]

in my experience i get this when i forget to defat .. but you're going STB so I don't know what to tell you

 

[steppa]

I'm confused though, on one hand I'm being told to add more solvent and on the other I'm being told to evaporate some. Out of curiosity what do you think would happen in each instance and what is your reasoning behind it?

stationdragon,

I'm not a chemist, so take this with a big chunk of salt:

Obviously something is pulled along with the spice, which causes the naphta to turn to jelly in the freezer. My intention behind adding more naphta is to lower the overall concentration of whatever causes the jellyeffect in the naphta. I guess that if one changes the ratio of the stuff that causes the jelly to ratio of naphta, the concentration of the stuff that causes jelly might be low enough for not being able to jelly up. At least that's my logic behind it.

Of course it would be better if we would be able to just not pull this stuff or neutralize it's effect in any way. But for this chemistry knowledge would be needed. :|

 

[stationdragon]

Steppa:

Thank you for your reply and for everyone's advice and patience with this.
Thank you for clarification on matters that I didn't understand fully.
After all the stress and confusion over all of this I have managed to save the DMT from this extraction, albeit a little lower than usual but I was prepared for that considering the numerous attempt I made at fixing the problem.
I found a post saying that goo is fine as an end result and that people get too hung up over crystals, so I decided to scrape my jars to loosen the precipitated material and pour through a coffee filter in the hope to save some DMT goo and try it out, but I was quite shocked when a bunch of yellow, sandy DMT was the end result.
The naphtha was still a little cloudy which isn't normally the case but I got 900mg from 100g of MHRB, which isn't too bad a loss considering what the spice was put through.
I got some more naphtha today so I decided to recrystallize for assurance of a clean product as I wasn't sure what else I pulled.
Strangely this time the solution stayed yellow instead of going clear with the junk falling to the bottom. After it had cooled I tilted the glass and there was a layer of orange/yellow material at the bottom but it wasn't noticeable until I tilted it and I was then able to siphon off the yellow naphtha into the next container before refrigerating and then freezing. Already there are pure white DMT crystals clinging to the jar. I'm going to continue transferring the jar between fridge and freezer for the next day to ensure good crystal growth. I'm expecting to end up with about 650mg/700mg of pure DMT. Not bad when you consider that I was going to sling the whole thing at one point.
Praise be to my tenacity.

Thanks again guys

 

[Grower]

In my latest extraction i didn't freeze precipitate the DMT, i just let the naphta evap in a large dish.
The result was a clear, sticky, oily substance that smelled strongly of DMT when vaporized.
I have pretty high temp inside maybe this was the factor in producing these results.
Actually i did freeze precipitate a small amount and got really white crystals but when i got the clear oily substance i decided to try dissolve all of the spice (crystals and clear oily thing) in hot naphta and try evap again.
This time i got clear oily substance again.
THis is a little strange as i got crystals last time i did this.
So now i have dissolved all of the clear oily substance in hot naphta and are in the process of freeze precipitate the DMT as it seems to be the only way to get white crystals for me.

This is really strange because in my last extraction i got nice crystals both from freeze precipitation and evapping the spice filled naphta.
Can my little higher than normal indoor temps explain that i get this clear oily form of DMT?
Anyone else have got this results?
Im quite sure the clear oily substance is very high concentraton of DMT, maybe almost pure.
I did an really good extraction procedure with many defat steps and vacuum filtrated my solution many times at various stages so it was free of unwanted stuff.

Is this clear oily stuff the gelly thing refered to in this thread?

Grower

 

[Grower]

So i tried freeze precipitate the oily DMT and when i took the crystallization jar out of the freezer it was full of very white crystals all over.
But as soon as temperatures got warmer the white crystals transformed back into clear, sticky, oily form again..grr......

So i must obviously do some kind of cleaning up procedure.
Maybe an water acid/base and following naphtha extraction will do it.
I don't want clear oil even if it is highly active, i want some crystals.
Very strange i get this as i did almost same extraction before with the same batch of acacia and got crystals after evaporate.
Only difference was this time i used 24% vinegar/acetic acid and before i used ascorbic acid.
And also batch size, this time was 4 times bigger.

So, back to studying cleaning up teks and recrystallization procedures...