Drying crystals using re-freeze question

[Atmozic]

Hi All,

So since I last posted I discovered that I had seriously bunk material that was never going to work, since then I swapped out to something better and instant success as far as getting to the point of drying. Basically the residue melted the minute I put it under the fan despite drying, Did some research and found that there could be a number of reasons but also a number of solutions - this one in particular caught my eye:

SWIMs crystals keep melting after freeze separation - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

so the technique calls for quickly draining the naphtha, then back in the freezer upside down and then the fridge (again upside down). What I'm wondering is:

- if you originally cover the freeze dish with plastic wrap, do you keep it on while drying upside down at both points (freezer and fridge)?
- if not, is there a risk of water getting into the freeze dish and contaminating the crystals?

Thanks for taking the time to look and for your replies.

 

[Emptiness]

When you quickly change from cold to warm it creates condensation. If i place me freezing crystal dish to dry it will always inevitably create some water residue... but so what? just leave it in the cupboard for a day or two and the water will have gone. Also, the water wont be everywhere. There will be spots where it is purely dry.
If you place any kind of uncovered naphtha in the freezer (even if in small amounts) it will evaporate and make your freezer smell nasty.

Dmt is polymorphous, its a crystal or a goo depending on the temperature and exposure to air. Try not to expose it to air for long periods and if you have go just scrape it up in to a container and place it in the freezer to maintain a solid consistency (obviously it will melt again once you take it out for a long period).

 

[MeecroHyperion]

SWIM has had disappointing experiences like this. In every case it was caused by lack of alkaloids in the solvent.

If there's nothing in the dish, there was nothing in the solvent. Whatever is melting is not what you're after, if you've kept everything below about body temperature.

You don't mention your method, but SWIM found the fastest way to test viability of MHRB was a mini STB at room temperature: stir 25-50g powder into 400ml water, 5g lye, 1g table salt stir, sit for 5 mins. Add 25-50ml naptha, stir for 30s and sit until separated. Add water if naptha does not separate. Pour naptha off into super-clean (acetone-wash if possible) glass petri-dish. Evaporate under fan until naptha milky. If this does not happen there is no point proceeding. Cover dish in freezer overnight. Crystals will form and stick to the glass. Pour off naptha in dish immediately leaving crystals. Do not filter. Leave dish open to dry. Freebase DMT will not melt at room temperature, but put it in the fridge if you want to be sure(but take out the food).

That at least will give you a baseline for your plant material. Being an absolute minimal process, the purity will be poor, but will give you an indicator of where you're at.

Good luck and Namaste.

 

[Atmozic]

SWIM has had disappointing experiences like this. In every case it was caused by lack of alkaloids in the solvent.

If there's nothing in the dish, there was nothing in the solvent. Whatever is melting is not what you're after, if you've kept everything below about body temperature.

You don't mention your method, but SWIM found the fastest way to test viability of MHRB was a mini STB at room temperature: stir 25-50g powder into 400ml water, 5g lye, 1g table salt stir, sit for 5 mins. Add 25-50ml naptha, stir for 30s and sit until separated. Add water if naptha does not separate. Pour naptha off into super-clean (acetone-wash if possible) glass petri-dish. Evaporate under fan until naptha milky. If this does not happen there is no point proceeding. Cover dish in freezer overnight. Crystals will form and stick to the glass. Pour off naptha in dish immediately leaving crystals. Do not filter. Leave dish open to dry. Freebase DMT will not melt at room temperature, but put it in the fridge if you want to be sure(but take out the food).

That at least will give you a baseline for your plant material. Being an absolute minimal process, the purity will be poor, but will give you an indicator of where you're at.

Good luck and Namaste.

Hi thanks for the reply. Just for reference I was using a modified version of Cyb's Salt Tek after talking to a few of the more experienced members. And yes the pulls came out a yellow-clear at first then after cooling/blowing turned instantly cloudy and crystals had already started to form on the bowl (after 1 hour in the freezer). So I'm pretty sure I have the alkaloids there.

 

[Atmozic]

SWIM has had disappointing experiences like this. In every case it was caused by lack of alkaloids in the solvent.

If there's nothing in the dish, there was nothing in the solvent. Whatever is melting is not what you're after, if you've kept everything below about body temperature.

You don't mention your method, but SWIM found the fastest way to test viability of MHRB was a mini STB at room temperature: stir 25-50g powder into 400ml water, 5g lye, 1g table salt stir, sit for 5 mins. Add 25-50ml naptha, stir for 30s and sit until separated. Add water if naptha does not separate. Pour naptha off into super-clean (acetone-wash if possible) glass petri-dish. Evaporate under fan until naptha milky. If this does not happen there is no point proceeding. Cover dish in freezer overnight. Crystals will form and stick to the glass. Pour off naptha in dish immediately leaving crystals. Do not filter. Leave dish open to dry. Freebase DMT will not melt at room temperature, but put it in the fridge if you want to be sure(but take out the food).

That at least will give you a baseline for your plant material. Being an absolute minimal process, the purity will be poor, but will give you an indicator of where you're at.

Good luck and Namaste.

Forgot to mention thanks for the technique to see if the material is viable or not that is a huge help. I'll give it a shot

 

[Atmozic]

Yep I think I stuffed up somewhere, too many plant oils?

 

[MeecroHyperion]

You're right - plenty of alkaloids!

Think you're 90% there. Lots of plant oils. They make SWIM very, very nauseous even to look at. Yuk.

The Acid part of a standard A/B extraction does remove some oils in waste naptha. There are other defatting techniques post-extraction like mini A/B's and "back-salting". They can help you clean up your extract.

SWIM found it convenient to remove the oils from MHRB before extraction. No post-processing. Your mileage may vary.

 

[Atmozic]

You're right - plenty of alkaloids!

Think you're 90% there. Lots of plant oils. They make SWIM very, very nauseous even to look at. Yuk.

The Acid part of a standard A/B extraction does remove some oils in waste naptha. There are other defatting techniques post-extraction like mini A/B's and "back-salting". They can help you clean up your extract.

SWIM found it convenient to remove the oils from MHRB before extraction. No post-processing. Your mileage may vary.

Thanks for that, if you look at my post at what I would call my first successful extraction I would say that oils were still present in the mix although the defat seemed to have prevented a great deal of it from coming across (for reference - what you are seeing above is extraction without defat).

One of the things I noticed in this particular attempt was that the crystals and alkaloids would either disintegrate or shrink phenomenally when attempting to dry, causing the yield to be next to nothing (and oily as you saw). Did SWIY happen to experience that? If so, what could be done to remedy if at all?

 

[MeecroHyperion]

Accepted wisdom says natural oils are not a problem with MHRB, but SWIM discards quite a bit of goo after pre-washing as per the link. It's a thick, solvent/oil goo, and smells horrible. Before adopting a pre-wash, SWIM used to see solid-seeming stuff disappear back into the yellow, like what you describe. But the alkaloids hadn't really made it across(just a little), and eventually came out later. Some early attempts were complete write-offs

For SWIM, oils were always a problem until pre-washing. Now, after that initial process, even crude STBs yield reliable crystals.

So maybe it's crystallization in lipid-rich solvent? SWIM can barely guess. Maybe still too much fat? Not much else in there.

Maybe the presence of too much fat retards crystal formation - maybe lipids fold into the crystal lattice at subzero temps. Then at room temperature the weak links disintegrate, along with your crystals? Maybe the presence of polar fats are changing solubility of DMT in the non-polar solvent? Maybe, maybe, maybe. Someone must know...

You're going to be the resident defatting expert before this is done ^_^

 

[Atmozic]

Crystallization in lipid-soaked solvent? SWIM can barely guess.

Maybe the presence of too much fat retards crystal formation - maybe lipids fold into the crystal lattice at subzero temps. Then at room temperature the weak links disintegrate, along with your crystals? Maybe the presence of polar fats are changing solubility of DMT in the solvent. Maybe, maybe, maybe. Someone must know...

You're going to be the resident defatting expert before this is done ^_^

that actually wouldn't surprise me if that were true, as you saw in the photos there was an abundance of stuff that was NOT DMT, so if that were the case it seems logical that it would retard the formation as it is in such a higher concentration. I imagine someone will know, and I will no doubt be closer to the answer myself after I do a Re-X as I am insanely curious as to what it will look like afterwards.

I may very well turn out to be a defatting expert, plenty of worse things to be an expert on. Who knows maybe I'll have some unique and useful info to contribute to the forum

 

[MeecroHyperion]

Sry was updating my post when you responded. Yes it sounds reasonable. As you say, there are certainly worse pursuits! Good luck and let us know how you go. Someone famous once said "The only way to fail is to quit trying. Death doesn't count."
Namaste

 

[Atmozic]

Sry was updating my post when you responded. Good luck and let us know how you go.

Thanks for that, I'll probably be keeping this thread as a bit of a journal and see what I can discover for myself. I didn't do a defat with this particular batch so maybe next time. Very hopeful that a Re-X will stabilise the goodies somewhat and put it to white but time will tell.

 

[endlessness]

Please note that the whole "yellow=fats" comments are a hypothesis, not a proven fact. The product is from MHRB, there is no evidence AFAIK that there are significant fats in MHRB. I've tested many different extracts from MHRB, from red-jungle to pure white/transparent and they were all pretty much all DMT, with very small amounts of other impurities none of which appeared to be fatty acids (as we've seen in phalaris extracts or others).

My own hypothesis in your case (considering your solvent evaps clean and isn't some impurity from the solvent) is that it is simply DMT, which as has been said before, is polymorphic so sometimes is yellow and gooey.

Goo/yellow doesn't have to be looked at as something bad, it can be just as active as white crystalline DMT.

So IMO you can simply scrape and rescrape the goo and let it air dry for a while to see if it hardens up, and then vaporize as-is, or make changa if it is too gooey and hard to store/handle. You can also re-x if you want, that is perfectly fine, but it is not strictly necessary.

 

[Atmozic]

Please note that the whole "yellow=fats" comments are a hypothesis, not a proven fact. The product is from MHRB, there is no evidence AFAIK that there are significant fats in MHRB. I've tested many different extracts from MHRB, from red-jungle to pure white/transparent and they were all pretty much all DMT, with very small amounts of other impurities none of which appeared to be fatty acids (as we've seen in phalaris extracts or others).

My own hypothesis in your case (considering your solvent evaps clean and isn't some impurity from the solvent) is that it is simply DMT, which as has been said before, is polymorphic so sometimes is yellow and gooey.

Goo/yellow doesn't have to be looked at as something bad, it can be just as active as white crystalline DMT.

So IMO you can simply scrape and rescrape the goo and let it air dry for a while to see if it hardens up, and then vaporize as-is, or make changa if it is too gooey and hard to store/handle. You can also re-x if you want, that is perfectly fine, but it is not strictly necessary.

**HAD TO EDIT AS IT WAS TERRIBLY WRITTEN**

Thank you for that, I was unaware that it was a hypothesis. As I'm trying to get to the point of crystals/freebase DMT. While the end result that I received has been educational and enlightening, I didn't want to stop at just this, I want to figure out what I could do to make it into the states that I want rather than accept the first result.

One of the things I want to learn how to do is back-salting as well, I'm not sure what the end result might be if I did. All part of the learning process and incredibly exciting.

 

[MeecroHyperion]

My own hypothesis in your case (considering your solvent evaps clean and isn't some impurity from the solvent) is that it is simply DMT, which as has been said before, is polymorphic so sometimes is yellow and gooey.

Goo/yellow doesn't have to be looked at as something bad, it can be just as active as white crystalline DMT.

Aha. Thanks for the info! In that case the yellow, oily-looking form makes SWIM vomit almost immediately. Solid extract precipitants with significant amounts of yellow look totally different under magnification compared with whiter samples. Curiouser and curiouser. Is there a way to isomerize into a preferred configuration for optimal crystallization?

SWIM had a pure sample turn bright orange after 6 months, didn't melt, was just as potent and non-nauseating. Oxidization?

Perhaps all she's been able to get is low-grade MHRB with higher-than normal organic components. All she knows is a naptha pre-wash solved all her problems, which were similar to Atmozic's. But talk is cheap:

If SWIM can find a local, discrete lab she'll save up and have her pre-wash goo tested and post the results here. That crap is nasty.

 

[endlessness]

Thank you for that, I was unaware that it was a hypothesis. As I'm trying to get to the point of crystals/freebase DMT. While the end result that I received has been educational and enlightening, I didn't want to stop at just this, I want to figure out what I could do to make it into the states that I want rather than accept the first result.

One of the things I want to learn how to do is back-salting as well, I'm not sure what the end result might be if I did. All part of the learning process and incredibly exciting.

That is totally understandable and I think you have a good attitude towards this. In the end, while the extractions lead us to a final product that we desire, if we think long term, each extraction is more than a means to a final product but rather a part of a learning process, where each time we learn another route and the key details associated with it, and next time can better tweak little details and do things better. Also with each experience, even (or specially) mistakes, we can then better help others who face them same issues as us.

So by all means do all the steps you want to do, re-x and clean up in different ways, bioassay the different products and see what you like best

Aha. Thanks for the info! In that case the yellow, oily-looking form makes SWIM vomit almost immediately. Solid extract precipitants with significant amounts of yellow look totally different under magnification compared with whiter samples. Curiouser and curiouser. Is there a way to isomerize into a preferred configuration for optimal crystallization?

SWIM had a pure sample turn bright orange after 6 months, didn't melt, was just as potent and non-nauseating. Oxidization?

Perhaps all she's been able to get is low-grade MHRB with higher-than normal organic components. All she knows is a naptha pre-wash solved all her problems, which were similar to Atmozic's. But talk is cheap:

If SWIM can find a local, discrete lab she'll save up and have her pre-wash goo tested and post the results here. That crap is nasty.

I don't think there is anything really in DMT extracts from mimosa that would make you vomit, and after testing different extracts from different MHRB batches I neither think it varies so wildly that you would have something so different in your batch, though I can't say that as a proven fact because of course I haven't tested every single batch on earth...

Two more likely (imo) possibilities occur to me, first is self suggestion (you didn't want yellow goo, it gives a bad visual impression if you don't know at first it is ok therefore you unconsciously expect it to be bad and give you bad experience), the second is related to smoking method and possible burned DMT and toxic/irritating by-products formed from combustion. How are you smoking/vaporizing it?

As for the orange DMT after storage, yeah some DMT does transform into DMT N-Oxide, but DMT N-Oxide transforms into DMT in the body according to Shulgin so it would be just as active (also if you wanted you could turn it back to DMT yourself with a zinc reduction).

As for lab work, I can help you forward to one to test for free, but it will take another month or so before they have the instrument back and running after some maintenance issues.

 

[Atmozic]

So maybe it's crystallization in lipid-rich solvent? SWIM can barely guess. Maybe still too much fat? Not much else in there.

Just an update, after using the RE-X process from Cyb I noticed a few impurities coming out, small dark flakes and such. Funnily enough there was VERY little oil and the coloration (which was quite a distinct yellow before) only lightened a few shades as I was dissolving the product. Will have some photos after it cools before I put to freeze I'd be very interested to see what you think.

@endlessness - thank you for your kind words, I'd be VERY interested to see your thoughts as well once it comes out of the fridge.

 

[Atmozic]

Here is the solution before putting in the freezer, hopefully it turns out well

 

[Atmozic]

So an update.....what a colossal failure, I tried RE-X, I actually got nothing out of it. Excuse the rant but hopefully the intention is clear, I honestly feel like I'm missing something very critical (whether it's in FAQ or some sort of assumed common sense step that I am honestly not picking up on), the frustration is genuinely due to a lack of success to achieve something seemingly very simple (simple to replicate, the skill is in tweaking) and the fact that I keep getting the same result despite trying to apply different methods as advice has been given and more reading/researching has been done. For the record I am reading the FAQ and I will freely admit that I have a hard time learning from just reading a book, actually doing and seeing with my own eyes and hands where I went wrong makes it much easier to understand and learn, as a result there could be things I'm reading but not interpreting, or reading and it's not "clicking" the way that it would with others.

So I did another batch, actually got crystals and then tried to RE-X....it actually came out oily wax....it actually went backwards.

So I tried another extraction, following Cyb's tek to the letter (as far as I understood it) except with a defat step as per his guide on the Max Ion Tek. For the current extraction the steps were:

1) Material
2) Vinegar (soak warm for 1hr)
3) Salt (soak warm for 30mins) - ok admittedly the tek doesn't explicitly call for that I wanted the salt to mix good and proper before adding the base after reading the Max Ion Tek and the explanation
4) Base (soak warm and mix gently for 2hrs), pH tested at 12.3
5) Added NPS and mixed (gently) as per tek guide
6) Extracted - came out milky :thumb_up:
7) repeated steps 5 and 6 (stopped at 3 pulls), still saturated
8) Did a gentle Evap on the dish to about 50% of the original volume, so far so good (pre-evap)
9) Placed in freezer
10) Checked 18 hours later - that's what was the result was (attachment - CURRENT)
NEXT STEP = keeping in the freezer and hope that the crystals start forming.

As far as Re-X, followed the Re-X guide and made sure to place in a larger container to avoid having too much naphtha as putting in a small glass did nothing but leave floaties. So while I can attempt to recover but I get the impression that I have messed up a batch, yet again.

*************************

As far as the floaties aside from the BEFOREREX (which I actually got crystals, I was thrilled) they always seem to do the same thing (including the technique of upside-down freeze after draining naphtha).

1). Result is a loose floaty mix
2). Drain and freeze upside down
3). Apply fan
4). what's there just vanishes, and I don't believe that it's a case of the solvent dissolving the goodies, but that whatever goodies are either non-existent or have been swollen by NPS and when dried - leave what's actually there which is very little or material wax/oil.


So with this in mind I've got a few things I need to ask and what's really frustrating is you can't just meet up and learn, so you have to describe as best as you can and hope you've disclosed enough to get help:

1) Change Tek
2) Is there something wrong with what I've described? (I really have no reason to have pride and hide a mistake)
3) Is there anything from the photos attached that would give some clue as to what might have been done wrong?

Again really hope that people understand the intent, and before saying "FAQ" just know I am HONESTLY trying.