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New recrystallization, because white spice is UNBELIEVABLE!!! Options
 
HippyDippy
#1 Posted : 3/13/2023 5:06:39 AM
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I am currently working on my first extraction's worth of spice. I decided to run 500g of MHRB bought as Tepezcohuite. I went with an A/B extraction and pulled roughly 1% spice, so about 5g. Now this 5g of spice was in various qualities across the board, as shown here:


This spice that I am going to recrystallize:


And the following is why I am going to bother with all the extra work...

I really didnt like the way it was so difficult to mess with the darker stuff, and I wanted to clean it up. Plus, having never done the spice before, I didnt know what I would enjoy smoking. I have read so many different trip reports across the spectrum of jim-jam to pure crystals, that I knew it was valuable to try the different levels of spice I came away with. This also meant that I needed to make some cleaner spice. Well, cleaner spice I made:


Now that I have tasted this white spice, I doubt I will venture back to to this dustier looking powder for myself. I can, however, see that it has a place and purpose. It is certainly not as powerful as the white powder, and therefore it is much gentler to give a spice virgin. I noticed that the duration was less than half also. This brown spice allowed me to enter hyperspace on more than one occasion, as well as a couple of waiting rooms, but it only lasted 4 minutes max with and afterglow lasting for about 15 more minutes. All of these trips were dosed between 50-70mg.

The pure white spice sent us to hyperspace for around 12 minutes each, with an afterglow lasting for another 20-30 minutes. One thing that I noticed when I first harvested this white powder though, it was much less dense than the brown. In other words, it seemed like a lot more, but weighed considerable less than I first thought. The whole pile of white goodness only weighed in at 240mg!!! This meant that a pile of white weighing 25mg was the same size as 50mg of the brown. My e-mesh is nearly at capacity with 25mg gently soaked into it. I am so glad that we didnt try to load 50mg of this white spice!! it is honestly SOOO much stronger than the brown stuff.

The main difference that we all took away from this white spice, was how the experience was so much crisper. The colors were much brighter, though still just as vivid. The brown spice seemed to make the same colors but in a darker shade. The Blastoff was also much smoother, and much faster. We all reached hyperspace within 30 seconds of finishing our hit. Each trip lasted longer than 10 minutes with the longest topping out at 14 minutes.

Now that we all had such a positive experience today, we decided to further process half of our brown spice. I have already redissolved 1100mg into heptane, separated the oils that fell out and am beginning to recrystallize. What am I doing different, and why is this relevant??? Well after much reading about recrystallizing, I figured out that the best way to make monster crystals is to go about it as slow is possible. So I took a styrofoam ice chest, and placed my electric tea kettle in it. I allowed my jar of heptane and spice to get as hot as practicable in the kettle, inside the ice chest with the lid on. This will keep the jar of heptane warm for hours, allowing it to cool as slowly as possible. My plan is to let it sit in the ice chest for 24 hours before I move it into the fridge. Then 24 hours in the fridge, and another minimum of 24 hours in the freezer.

We should have some awesome shards after all that, eh?
 

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Jees
#2 Posted : 3/14/2023 3:22:47 AM

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Hi,
the yellow/brown/oily-dmt likely needs a higher vaping temp compared to the white. Your e-mesh might have lesser trouble getting the whites evaporated? This might contribute to the differences noticed.
 
Loveall
#3 Posted : 3/14/2023 3:55:45 AM

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Jees wrote:
Hi,
the yellow/brown/oily-dmt likely needs a higher vaping temp compared to the white. Your e-mesh might have lesser trouble getting the whites evaporated? This might contribute to the differences noticed.


I agree and have experienced this effect first-hand.

The yellow/oily DMT is also harder to dissolve in naphtha - FYI.
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HippyDippy
#4 Posted : 3/14/2023 10:20:27 PM
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PROBLEM! As I said previously, I dissolved 1100mg of spice into what ended up being 40ml of heptane. I used this amount because it was so thick, that nothing was separating. This pic is with only 20ml:


I let it cool enough that stuff settled on the bottom of the jar, and I pipetted the liquid to another jar. I let all of this heat back up 1 more time, because the transfer jar was cold, inside the ice chest. Once hot I turned off the kettle, and left it to slowly come up to room temperature as slowly as possible.

Upon checking it the next day, to remove the kettle and place the whole chest in the fridge, I noticed that my previously yellow but clear liquid had again separated into 2 layers. The top layer was an even lighter shade of yellow clear liquid, while the bottom layer was an opaque mess of white sediment. Here is the thing though, the layers are almost perfect halves of the fluid. So 20ml clear and 20ml sediment. It truly looked like I had done another water wash.


Whats the deal with that?

So at the direction of the Mrs., I again pipetted the clear liquid off the opaque into a clean jar and am treating them both as if they have spice in them to precipitate out. I separated the layers yesterday, and left them in the fridge for 24hours. Today I found some crystals growing in the clear liquid, and some "chunks" growing in the sediment. I am likely going to evaporate the sediment jar, and try to re-x again with naptha this time.



Edit: Clarification about 40ml heptane, and added 1st pic
 
Toshido
#5 Posted : 3/14/2023 10:47:49 PM

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Excited to see the pictures tomorrow. I'll reiterate the wonderful ease of use with 100mL beakers though. The spout makes it easy to decant. No need for a pipette.
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HippyDippy
#6 Posted : 3/15/2023 12:11:31 AM
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widderic wrote:
Excited to see the pictures tomorrow. I'll reiterate the wonderful ease of use with 100mL beakers though. The spout makes it easy to decant. No need for a pipette.


I got my crystallization dish today, no spout though...
 
downwardsfromzero
#7 Posted : 3/15/2023 7:42:39 PM

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HippyDippy wrote:
So 20ml clear and 20ml sediment. It truly looked like I had done another water wash.


Whats the deal with that?
Plant particulates in your naphtha, maybe, just based on the visual appearance. Presumably it came through with the initial product that you put into the recrystallisation. This raises the question of what exactly you did with the pulls from your initial tepezcohuite extraction. My thinking is that if this isn't simply bark powder (which you shouldn't have allowed into your product...) then there's some kind of weird tannin-like material in the bark. 1% is a remarkably high yield for tepescohuite, btw. really makes me wonder about your source material.

What kind of residue was left by the brown material that required 50 - 70mg per dose? That's sounding more like it has inactive impurities than it simply requiring a higher vaping temperature.




“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
 
HippyDippy
#8 Posted : 3/18/2023 12:30:27 AM
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downwardsfromzero wrote:
HippyDippy wrote:
So 20ml clear and 20ml sediment. It truly looked like I had done another water wash.


Whats the deal with that?
Plant particulates in your naphtha, maybe, just based on the visual appearance. Presumably it came through with the initial product that you put into the recrystallisation. This raises the question of what exactly you did with the pulls from your initial tepezcohuite extraction. My thinking is that if this isn't simply bark powder (which you shouldn't have allowed into your product...) then there's some kind of weird tannin-like material in the bark. 1% is a remarkably high yield for tepescohuite, btw. really makes me wonder about your source material.

What kind of residue was left by the brown material that required 50 - 70mg per dose? That's sounding more like it has inactive impurities than it simply requiring a higher vaping temperature.



I admit, there was a fair amount of leftover residue when we first smoked the stuff I am trying to recrystallize now. We were also using oil burner pipes, which we have happily graduated from to e-mesh.
I was very careful however to make sure that none of the based-bark material made its way into my naptha wash. One thing that I didn't do however, was perform a water sodium carbonate wash on my initial naptha pulls. I have only water washed some recrystallizations I have done.

A picture of my initial naptha pulls:


It has had a pretty dark color from the start. I think this may be due to my use of heat during my extractions. I kept my base solution warmed in a crock-pot of hot water while I did all of my naptha pulls.

I don't remember where I read about the content of spice in tepezcohuite, but I admit I may fully be wrong. Do you know where I should look to find that information? Also, being my first time buying root bark, I didnt know where was a reputable source. I cannot say here where I purchased, due to rules and such, but I'd be happy to discuss with you in a PM. Perhaps you could steer me in the right direction.

EDIT: I forgot to mention, I dried out my precipitated spice. It was a pretty dismal yield at only ~113mg from a starting weight of ~1100mg. And not very clean!!


I was certainly hoping for quite a bit more than that, but I am still going to see whats up with all the sediment. After a bit having splashed out while "boiling" in the vacuum chamber, and a fair amount still stuck to the side of the jar, there was ~390mg of wierd looking sediment.
 
downwardsfromzero
#9 Posted : 3/19/2023 9:19:42 PM

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What is the exact procedure that you use when performing what you refer to as a recrystallisation?

The weird sediment in the last picture looks as much like inorganic salts as anything, although it's impossible to do a chemical analysis of a picture on the internet.

The naphtha in that Erlenmeyer flask has a load of suspended watery material which was likely the source of much of the contamination.




“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
 
HippyDippy
#10 Posted : 3/20/2023 11:05:14 PM
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downwardsfromzero wrote:
What is the exact procedure that you use when performing what you refer to as a recrystallisation?

The weird sediment in the last picture looks as much like inorganic salts as anything, although it's impossible to do a chemical analysis of a picture on the internet.

The naphtha in that Erlenmeyer flask has a load of suspended watery material which was likely the source of much of the contamination.


To this jar I added 10ml of naptha.
The jar was sealed and placed in a hot water bath, until everything was dissolved.
Then left on work table until the jar and contents reached room temp, which currently is in the 50-60's. Wait until a layer of anything shows up on the bottom, (I say a layer of "anything" here because I have seen dark oily settle out, and I have seen tanish/whitish sediment. Never have I seen black soup like my base solution) then pipette off the yellow naptha into a clean jar.
Place the yellow naptha into fridge for 24 hours, then freezer for 24 hours.
Pipette off remaining naptha and place jar with crystals into a vacuum chamber to evaporate any remaining naptha.

Is that not a pretty standard re-x tek?

EDIT: Only answered one part of quote
The naptha in the flask did have an emulsion layer in it when I took that picture. However, the emulsion was completely separated prior to me removing the naptha
 
Toshido
#11 Posted : 3/20/2023 11:24:45 PM

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I made a pic by pic tutorial on Recrystallization and it's fairly simple compared to what you're doing. I think your issue may be temperature related while doing water washes, hard to tell without knowing your full step by step process. Mistakes can be made at any turn.

Re-X

Just scroll down past the TEK where the Re-X tutorial is.
🌳👨‍🔬🌳 - My A/B Hot Plate TEK - 🌳👨‍🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
✴✴✴ - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
downwardsfromzero
#12 Posted : 3/20/2023 11:29:49 PM

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Thanks for explaining. Yes that's a standard re-x in this instance. It seemed best to ask because occasionally some individuals have a misapprehension of what a re-x is and/or not understand the principles behind it. Troubleshooting sometimes entails asking or stating the obvious - I've seen all sorts of nonsense over the years Big grin

Is there anything that you did which you may have overlooked? Otherwise, besides just scratching my head I'm still inclined to chalk this one down to use of tepescohuite - which I understand to be the trunk bark - rather than jurema, which is the root bark.

We'd be keen to hear how it goes with a few more extractions from your material as yield reports from trunk bark extraction are decidedly thin on the ground.




“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
 
HippyDippy
#13 Posted : 3/21/2023 12:03:34 AM
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downwardsfromzero wrote:
Thanks for explaining. Yes that's a standard re-x in this instance. It seemed best to ask because occasionally some individuals have a misapprehension of what a re-x is and/or not understand the principles behind it. Troubleshooting sometimes entails asking or stating the obvious - I've seen all sorts of nonsense over the years Big grin

Is there anything that you did which you may have overlooked? Otherwise, besides just scratching my head I'm still inclined to chalk this one down to use of tepescohuite - which I understand to be the trunk bark - rather than jurema, which is the root bark.

We'd be keen to hear how it goes with a few more extractions from your material as yield reports from trunk bark extraction are decidedly thin on the ground.



From my understanding what I bought was supposed to be root bark, PM sent btw. I was already planning to do another extraction on what I have left, since I still have another 500g. I will only be running 100g this time though, in an effort to improve my extraction procedures.

There is also the possibility that I have gotten every last crumb of spice out of this material. It was some nasty, nasty stuff to begin with. I promise there was no base solution in this jar at all, this was just the insane amount of goo I was left with after evaporating 500g worth of starting root bark.


I am also thinking that my lack of filtration between acid and base steps may have ultimately screwed me. I missed that step when I was reading all the teks first. Or I just thought it wasnt ultimately important, I'm not sure which.

I absolutely will be doing a "fridge settled" decanting after my acid step next time.
 
Toshido
#14 Posted : 3/21/2023 12:37:37 AM

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HippyDippy wrote:
what I bought was supposed to be root bark


Bought? You mean harvested right?
🌳👨‍🔬🌳 - My A/B Hot Plate TEK - 🌳👨‍🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
✴✴✴ - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
HippyDippy
#15 Posted : 3/21/2023 4:48:40 AM
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widderic wrote:
HippyDippy wrote:
what I bought was supposed to be root bark


Bought? You mean harvested right?

"Harvested"...
 
 
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