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Issue with recrystallization ( oiled and wet )

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watermelon555

Rising Star
Hello everyone,

I have some issues to re-X my DMT from MHRB :

When I put the dish out from the freezer, after about 1h in front of the fan the spice/dish is still "oiled" and "wet" like the pictures and smell Heptane. (Even if I wait days/ or a week)



I make extraction for about 2 years and I really don't understand what happenned and how to avoid that. Sometimes the spice is dried after 30mn and the smell was good, sometimes not.


- Got the same issue with Naptha. that why I tried n-Heptane.
- I did a test to make sure that the n-Heptane is clean.
- I tried Acetone wash, same issue.
- I tried to Re-X 3/4/5 times, same issue.


If anyone can help me to save this spiece and understand what happened it would be awesome.
 
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Just a side question out of curiosity, from the moment you encounter more oil in your results, have you concentrated your extracting volumes somehow, like working in smaller concentrated volumes to pull on? Or using more bark in same volumes to pull on? Or using more salt (NaCL) if you use that kind of tek. Or using more base and/or stronger base? Thanks.
Very cute crystals btw.

PS:
watermelon555 said:
...I have some issues to re-X my DMT from MHRB ...
Click to expand...
If you use a pyrex pan in the freezer with a layer of naphtha as in the pics you provided, this is usually called 'crystallization'. The term re-X (re-crystallization) is when like 1gr of deems get redissolved in only 30ml of warm naphtha, and that tiny volume get's freezed.
 
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Thank you for your answer,

I used Acid to bas tek : Cybs' Hybrid ATB 'Salt' Tek - DMT-Nexus Wiki
I use 50gr of MHRB, 30gr of salt and 50gr of base and distilled water on each bottles.

Here is where I bought the n-Heptane : Heptane 99% min. ACS (n-Heptane) 3x1L **Free P&P** | eBay
Not sure to find where I can find the CAS number, here are the sticker on the bottle : https://ibb.co/zPs015V

Note - I have the same problem using Naphta.


-> Jees

It was a Re-x ( Maybe the 5th time ) I use a Pyrex for my Re-x ( Or a beaker ).
- This is not recommended ?

I put my spice in a beaker with very hot haptane ( or Naptha ), used a hot plate magnetic stirrer to do that.
- About 90/100°

Then I put the hot solvant/spice on a Pyrex with a plastic film, and this go to the freezer after about 1/2hours for at least 12/18 hours.

I have to make ReX because the "crystallzation" is going wrong the first time, oiled and smell very bad... SO I have to Recrystallize again and again, but it's still wrong I really don't get it.


Thank you for your help.
 
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Nothing wrong with doing multiple crystallization one after the other. I guess you called it re-X but what I wanted to say was that the term "re-X" is usually reserved for recrystallizations of a lot of deems (e.g. 1 gram freebase) in very small volumes of warm naphtha bordering saturation of the naphta, like 30 to 40 ml of naphtha only. If you use a pyrex dish with more naphtha and do this multiple times after each other, it's in public nomenclature not considered "re-X", rather "crystallizations". It's name picking only :oops:
 
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Are you sure the oil is bad? DMT can look like that sometimes. Of course if smells like solvent, I would be concerned. However, I have to say the pictures look ok to me.

Did you evaporate a fresh sample of your heptane and other solvents? If they leave no residue you should not have any in your DMT either.

You may be able to revert some of the oil to xtaline DMT (or also remove it if it is a contaminant) by dissolving in acidic water and basing/pulls again (maybe minimize time as a base and avoid NaCl). These pulls will be very easy compared to stuff with plant material. See if there is less oil.

Have you seen this example? 100% oil was changed to xtals. The orange oil was DMT the whole time, just wearing "different clothes".
 
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Jees, Thank you, I get it now!
So yes, today I tried a Re-x this time and this was again wrong : https://ibb.co/M9jd0G1

I put about 40ml of very hot pure Heptane with about 2.5gr of spice.

No need freeze precipitation, I had quickly some really beautiful white crystals, but still, they smell Heptane after hour and hour in front of the fan.

-----

LoveAll, Thank you very much for your feeback and for this post, this sound really interesting. So do I need to Re-X it into hot acidic water ? Where can I find this ?

- Yes I evaporated a fresh sample n-heptane and it was really clean.
This is the Heptane I bought : Heptane 99% min. ACS (n-Heptane) 3x1L **Free P&P** | eBay

- Yes the final spice smell solvant again. Not possible to me to smoke that. I really don't understand where I'm doing something wrong. It looks like a lottery to me and I can't save the dmt I don't know why.
Sometimes I would like to try some extraction with natural product, I heard with Limonene it works fine.


I do extractions and smoke DMT for about 2 years, I can smell it when it's wrong now ! Maybe I have to try without Salt or change the base.

By the way what do you do with the yellow yield with the Re-X. Changa ?

Thank you, I hope to understand more what happenned.
I learn a lot from this forum.
 
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Heptane evaporating clean is a good sign. You can also rinse the containers you use with it and evaporate to test the containers (maybe one of your containers leaches oil somehow?). If you are using a fan, I would also flow air from it over fresh heptane and see if the oil shows up (it shouldn't, just checking for any possible source). If you cover with lids, add those to the evap test, etc. Essentially add parts of your extraction to the fresh solvent evap test to try to figure out where the oil is coming from.

If some foul smelling oily contaminant got in there that persists after re-X, and your tests show that an empty "re-X" using only fresh solvent (no product) has no oil (meaning your equipment is not the source), I would do a mini A/B. Simply dissolve your xtals in a small ammount of vinegar, wait at least a day to see if anything settles (decant if yes), then base with NaOH. Gentle conditions, pH 12 is plenty, the concentrated clean water solution will become milky, and immediately pull with fresh solvent. Then follow the usual partial evap/freeze to get xtals (you can test this with fresh hexane first as described above to make sure no oil is coming through your materials,). Use only glass containers that are very clean. Make sure lids are not breaking down, etc. Maybe you have done all this already, but if you haven't that is what I would do next.

Best of luck 🤞
 
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shroombee said:
Your n-heptane seems fine. Scroll down to the Hazard Information on the listing and it says the CAS is 142-82-5.

How about cleaning up the crystals with ethanol?
Click to expand...


Thank you for your answer, do I need to use Ethanol the same way we use Naptha/Heptane for Re-x ?



Loveall said:
I would do a mini A/B. Simply dissolve your xtals in a small ammount of vinegar, wait at least a day to see if anything settles (decant if yes), then base with NaOH. Gentle conditions, pH 12 is plenty, the concentrated clean water solution will become milky, and immediately pull with fresh solvent. Then follow the usual partial evap/freeze to get xtals (you can test this with fresh hexane first as described above to make sure no oil is coming through your materials,). Use only glass containers that are very clean. Make sure lids are not breaking down, etc. Maybe you have done all this already, but if you haven't that is what I would do next.
Click to expand...


Yes, the smell is still here, I didn't make any acid base yet. I will try today.

I don't want to do any mistake for this :

- about 30ml of vinegar for 24 hours at room temp in a clean beaker ?
- How much salt ?
- How much base ?
- Do I need to use the hot plate of my magnetic stirer to do the pull when I put Heptane ?


Thank you so much for your help. I didn't thought about making a Mini Acid Base.

Will let you know!

love you all.
 
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Use minimal acid to dissolve all, no more. Water is no problem as water helps the concentration down, also this time please try to use no salt and minimal base to get to 12 only no more. The aim is to have as less concentration of various stuff (ions) as possible in the volume you pull on.

These directives are experimental and you might help in getting more experiences with lower concentrations, to see it this helps avoiding oil/waxy results.

It would be good to not change your pulling strategy itself. If there is a change in result then we could narrow down what factors were responsible for the change in results if any.

Happy trials :thumb_up:

PS: experiences show fundamentally lesser oil when keeping concentration down, just a week ago. Yield was only 1.1%, but there were more changes done (1 month bark cold acid soak, no boils) so have to figure out what did exactly what.
 
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Jees said:
Use minimal acid to dissolve all, no more. Water is no problem as water helps the concentration down, also this time please try to use no salt and minimal base to get to 12 only no more. The aim is to have as less concentration of various stuff (ions) as possible in the volume you pull on.

These directives are experimental and you might help in getting more experiences with lower concentrations, to see it this helps avoiding oil/waxy results.

It would be good to not change your pulling strategy itself. If there is a change in result then we could narrow down what factors were responsible for the change in results if any.

Happy trials :thumb_up:

PS: experiences show fundamentally lesser oil when keeping concentration down, just a week ago. Yield was only 1.1%, but there were more changes done (1 month bark cold acid soak, no boils) so have to figure out what did exactly what.
Click to expand...

I second all this. Would only add to pull quickly, minimize the time dmt is in water as free base. Based on experiments (and I could be wrong, this is just what I have seen) I think time in the watery base is when DMT agglomerates and comes out as an oil at the end. Actually, if you let it sit in the basic water long enough you may see an oil starting to form at the top of the water. Salt, and/or very high pH (both contribute to ionic stenght) seem to accelerte this agglomeration. Less excess vinegar will also result in less salt after neutralizing. There is a sweet spot though, because if too dilute and low ionic stenght, the pulls are less efficient.

My best results are when basing the mini A/B gives a milky white smooth color. If yellowish or clumpy, there is always some dmt oil at the end.

There is also the TEKs. In the "max ion" approach, a few grams of DMT are diluted all the way to a liter of water, and I believe the ionic strength is ~10% which gives food results. I think we can also get good results when DMT is more concentrated, but then we need to minimize the ionic stenght. If DMT is concentrated (mini A/B) and ionic stenght is high, I think we cross the line and start making oil. If DMT is dilute (plant soup) and ionic strength is low, them the we go too far in the other direction and pulls are innefficient.

watermellon55, while you are more concerned about non-dmt oil, perhaps reducing the dmt oil may help clarify your situation.
 
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Jees said:
Use minimal acid to dissolve all, no more. Water is no problem as water helps the concentration down, also this time please try to use no salt and minimal base to get to 12 only no more. The aim is to have as less concentration of various stuff (ions) as possible in the volume you pull on.

These directives are experimental and you might help in getting more experiences with lower concentrations, to see it this helps avoiding oil/waxy results.

It would be good to not change your pulling strategy itself. If there is a change in result then we could narrow down what factors were responsible for the change in results if any.

Happy trials :thumb_up:

PS: experiences show fundamentally lesser oil when keeping concentration down, just a week ago. Yield was only 1.1%, but there were more changes done (1 month bark cold acid soak, no boils) so have to figure out what did exactly what.
Click to expand...



Ok so ! I tried to quick mini acid / base. Let me show you the pictures.
I don't have any test ph, do all do the jobs ? I will buy one.

As you say, just a bit of vinegar - water - base - clean heptane - used my magnetic stirrer and pulled this...



Looks better, still yellowed.. I will put it on the freezer after 1 hour. Will let you know tomorrow with a pictures out from the freezer.

Looks like Acid to base is better without salt ? What do you think ?


Here's what I get just on the top of base but not on heptane.. Is that impurities ?

 
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A little yellow is fine. Are you seeing any of the bad smelly oil you are worried about?

That stuff floating at the top could be dmt oil. You may need to heat up the naptha (warm water bath, no direct flame). It may crash out of Naphtha as an oil, but it should smell like dmt and be ok to use. If so, it may have formed after the acid step if you added too much base. Or maybe the acid step was not long enough to break it all up, I don't know.

Also, is the water still milky? You should pull until the milkiness dissapears.

Usually, the dmt oil crashes first if you keep on eye on it, and then the xtals. The dmt oil is less soluble in the solvent. It also dissolves last during re-X (I think I've mistakenly thrown DMT away during re-X in the past because of this).
 
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Loveall said:
A little yellow is fine. Are you seeing any of the bad smelly oil you are worried about?

That stuff floating at the top could be dmt oil. You may need to heat up the naptha (warm water bath, no direct flame). It may crash out of Naphtha as an oil, but it should smell like dmt and be ok to use. If so, it may have formed after the acid step if you added too much base. Or maybe the acid step was not long enough to break it all up, I don't know.

Also, is the water still milky? You should pull until the milkiness dissapears.

Usually, the dmt oil crashes first if you keep on eye on it, and then the xtals. The dmt oil is less soluble in the solvent. It also dissolves last during re-X (I think I've mistakenly thrown DMT away during re-X in the past because of this).
Click to expand...


Thank you for your reply.

Here's my crystal from mini acid/base, 2.5gr ! :



No oil anymore ! But have to put them about 5 hours near a fan, still smell a tiny bit heptane.... Not much as before.

How long do you wait to this smell totally disappear?
Sometimes I feel like heptane is traped with dmt.

I'm a bit anxious with that, I smoke DMT for about 2 years, had already bad experience smoking naptha, that why I take care of my extraction.

Thank you all !
 
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I don't know why for some reason it happen (like 50%) when I'm doing a Re-x. Looks really easy to do, still have to learn I guess.

Maybe I put my hot plate from my magnetic stirrer too high, I don't know. Smell never leave the DMT.


If you smoke naptha, you feel that quickly it will be not a normal trip. You need to spit a lot like gaz is in your lung and you are far away. Really not a good moment.


That why I would like to learn how to make extraction 100% natural one day.
 
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