Help! How to recover from failed re-x

[Digi123]

Hi

Just tried to do a re-x on some off-white spice and it seems to have gone horribly wrong but I'm hoping it can be rescued

Will explain what I did.

A bowl was filled with hot water from a boiled kettle. 3.5ml of lighter fluid was added to a glass and placed into the water bath for ~5mins. 0.381g of slightly off-white spice was then added to the glass. This was then mixed using a pipette until all of the crystals were dissolved (yellow goo was observed settling at the bottom of the solution). When thoroughly dissolved, the solution was transferred to a shallow dish using a pipette. The yellow goo was discarded (maybe should have kept it). The dish was then put into the freezer for 24 hours.

You will see the pictures below of the mess that resulted in the tray after 24 hours

The dish had been in the freezer as it had a few small crystals stuck to it from a previous batch which I didn't want melting. When the solution was being transferred after removing the goo I could see it instantly turning very white as soon as it came into contact with the dish as it was cold so it forced it to crystalise & it was super-saturated anyway.

As soon as I'd put it into the dish I had a feeling that was a bad move! Seems obvious now and I really should have known. If anything, a warm dish that could be cooled to room temperature slowly before being put into the freezer would have been a much better idea!

I'm also wondering if I would have been better using more solvent? Maybe 3.5ml was not enough, after reading some re-x teks today they seem to advise ~20-30ml per 1g of spice.

I would appreciate it if anyone has any ideas for how I can somewhat salvage this

Thank you


p.s - this is written from memory (which is generally not so great considering the amount of weed I smoke on a daily basis ) and I've got that feeling I've missed something out, not sure what though, could be nothing, I get that feeling all the time . Really should start writing down notes as I go along with these things...

EDIT: Aha!! I know what that thing was that I'd forgotten before The 3.5ml of solvent used for the re-x was lighter fluid that had previously been used for 1, possibly 2 pulls and was yellow, not clear. Thinking now that clean solvent should be used for re-x and if possible something a bit better than lighter fluid?

EDIT2: White spots in the photo's are just the camera flash.

 

[endlessness]

I dont know if I understand it.

First of all yeah, that amount of fluid might not have been enough. Lesson 1 is not to throw anything away till you have your final yield.

But in any case a part of your alkaloids would def be in the solvent. Then you added to a cold container and it crystallized immediately? So whats the problem? Is that image with or without solvents? Can you scrape it up and get it together? And if its a goo, with some scrapping and moving around it should harden up. You can always recrystallize again if you want.


edit: And yeah for sure clean solvent should be used for recrystallization, isnt your purpose to clean your product? Why would you use dirty solvents then?

If I understand your post then yeah you probably lost quite some spice to the yellow you threw away, and now you have some more dirty stuff from the reused solvent, that you need to recrystallize again.

 

[Digi123]

Thanks Endlessness. I saw you reading as soon as I'd posted and inside I went "yay"

Understand quite why it hasn't worked, or why I was silly enough to use dirty solvent to try to clean crystals? xD

Lesson 1 noted

Yes pretty much. I wouldn't say it had crystallised completly but it went totally opaque, totally white and looked very viscous. I didn't really look at it for long. I thought if it's started to crystalise I should just get it in the freezer asap.

The picture is with the solvent. So evaporate, scrape & dry, see what's there, re-x again?

Yea I think I've lost a good bit with the yellow too, it looks a good bit less this time.

Oh well, still learning, these things happen!

Thanks for the quick reply

 

[Digi123]

Could some of the yellow goo that was left in the glass that I discarded have been liquid DMT that was not dissolved in the solution? I'd thought at the time that it would just be oils etc otherwise I would have added more solvent

 

[Trips]

So your spice was a freebase when you added the lighter fluid? It is possible that the yellow goo was indeed spice that had absorbed a little solvent, but not enough to dissolve. It is important to keep polarity in mind when doing these extractions. You say you thought it could have been oils, but these would likely dissolve in your lighter fluid, which is essentially a very light oil. Use clean solvents for recrystallizations. And ideally for subsequent pulls too. Or do multiple washes with one round of lighter fluid, and multiple washes with fresh stuff. Scrape up the crystals and try again.

Try to do your recrystallizations in a deep, narrow container, preferably with a small opening (like an erlenmeyer- as I assume you don't have a reflux condensor) or... a little jar. Put the lid on. You want to avoid having solvent evaporate during recrystallizations, or as it evaporates, it will just drop out nasties on to your crystals.

 

[Digi123]

Hi Trips

Yes, the spice was freebased. Ok thanks, I hadn't realised the oils would dissolve. I'm looking for alternative solvents for recystallisations but they're hard to find in the UK.

Or do multiple washes with one round of lighter fluid, and multiple washes with fresh stuff. Scrape up the crystals and try again.

Sorry I'm not sure what you're meaning here. By washes are you meaning pulls or recrystallizations? Clean solvent for a pull then precipitate, filter and use the same solvent again for a few pulls before changing solvent, or do you mean using a clean solvent to recrystallize, then using that same solvent to recrystallize another batch? Possibly both even?

Nope, I have nothing more narrow than a smallish glass. I have the morning off tomorrow so I can nip into town and find something I'm sure.

Thanks Trips

 

[Digi123]

It seems to be drying out quite well. It's not as bad as I thought it was going to be. From the first pictures I thought it was going to be a little bit of goo rather than actually dry out

Need to wait until tomorrow before I have clean solvent to re-do

 

[q21q21]

That looks NICE.

Personally I think that is beautiful and likely very clean. The reason is based on a theory which I plan to put into a neat little thread but I'll just put a quote from a post I made recently stating it

You know I have stated this in my tek and a few time in the post

I STRONGLY believe that the yellow in spice like that (but not the brown in dirty spice, that I'm pretty sure people accept as lye-soup in naptha) is JUNGLE DMT, that red stuff that dissolve really well in d-limonene and xylene but also somewhat in naptha too

So it totally makes sense that having the crystals precipitate with some jungle mixed in or coated or whatever that you would get such a nice yield.

Sure it might be plant fats but I know that in my experience 20mg of white is EQUAL TO OR LESS THAN 20mg of yellow spice which suggests otherwise.

In either case, pretty spice, nice extraction, pleasant journeys.

So by re-xing to WHITE I believe you would not be gaining purity but losing jungle!

 

[DoctorMantus]

It seems to be drying out quite well. It's not as bad as I thought it was going to be. From the first pictures I thought it was going to be a little bit of goo rather than actually dry out

Need to wait until tomorrow before I have clean solvent to re-do

What a beautiful pile of goodness.

 

[rhave]

how much spice made it through? It's likely the yellow oil contained some of your product. In my experience plant oils dissolve DMT at least as well as naphtha. It may have even been mainly molten DMT. Generally when recrystallizing you try to use enough solvent to get everything into solution at high temperature, if your spice was freeze precipitated originally there should be nothing in it that isn't soluble in naphtha and if your lucky the stuff that isn't DMT is in there in small enough quantities to remain in solution at whatever temperature you freeze it at. Slow cooling is also key as otherwise the crystals are small with a porous structure which traps solvent and whatever is dissolved in it.
For low boiling solvents i usually boil until it begins to become cloudy then add just enough solvent to make it clear before allowing to cool. With naphtha it's a bit more guess work as I usually don't want the product getting as hot as naphtha boils.

 

[Digi123]

how much spice made it through?

Ended up with 377mg (from 381mg originally), slightly yellow as seen in the previous picture. I guess the yellow is just oils or something from the un-clean solvent I'd used to re-x or oxidisation during freezing. Didn't really lose very much, although if some DMT was lost the weight was maybe regained by picking up oils from the solvent.

I've left it as it is rather than re-x it as it's ok. Deffinately going to continue playing around though with my next batch, much learning to be done

I can't really heat my solvent very high yet as I have to just use a kettle of boiling water. I have a gas cooker but planning on acquiring an electric hot plate sometime soon so that I can get a better bath on the go

if your spice was freeze precipitated originally there should be nothing in it that isn't soluble in naphtha and if your lucky the stuff that isn't DMT is in there in small enough quantities to remain in solution at whatever temperature you freeze it at.

The solvent always retains a hint of yellow after freeze precip so there must be something still in there, wether it's DMT or oils, or a mix of both. I evapped down some old, used solvent the other day and there are crystals in there, just with a lot of gunk.

I haven't really decided on what I'm going to do with it yet, It's only a very small amount (around 50mg or so, not weighed it yet) so it doesn't really matter if it gets lost, the knowledge is more valuable

NaCO3 wash is only helpfull at removing lye/water solution right? Doesn't help for anything else?

I have activated carbon (AC) granules there, I'd think I might melt it down, wash with some AC, then do a re-x, just to see what happens Or maybe I'll re-x 1st just to see what kind of difference it makes, then, if it's not much improved, try the AC.

Slow cooling is also key as otherwise the crystals are small with a porous structure which traps solvent and whatever is dissolved in it.

Yea slow cooling for sure. I'm not sure what temp my freezer goes to, I put a thermometer in there which apparently goes down to -40c but it seemed to get stuck as soon as it hit 0c . Deffinately going to warm the glass tray to at least room temperature before putting the DMT solution in there, maybe put it in the fridge for a few hours, then into the freezer. That's about as slow as I can cool it, wish I had a seperate mini freezer I could make reduce by 1 degree C every hour or something