Animistic
Titanium Teammate
BTW @Transform if he backsalted shellite to begin with surely the stuff would come back into fresh shellite if it were another alkaloid rather than a by-product of the lye/vinegar, right?
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Cyb tek HELP! Currently in the middle of extract..
- Thread starter SunshineMaker
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Just a result of racking my brains on what it possibly could be, based on what's happened in the extraction so far. Don't let that stop you - I'm far from being the fount of all knowledge; I just rather enjoy thinking about chemistry.
Huh? Did I misread something? If the insoluble white crystals came out of a vinegar wash on the shellite-pulled material I'd have to think again. My mind was resolutely on the tracks of believing this was about avoiding the evaporation of a xylene pull. If I got that wrong, I should definitely just go to bed!
Animistic
Titanium Teammate
@Transform (highlights mine)
I mentioned xylene as a way to extract from the original base soup to see if there's something the shellite didn't extract. It seems to me he backsalted his shellite pulls.
If you need to question it you probably should goto bed
I mentioned xylene as a way to extract from the original base soup to see if there's something the shellite didn't extract. It seems to me he backsalted his shellite pulls.
If you need to question it you probably should goto bed
uh wut? Was that "pop" the sound of my credibility disappearing? Off to the optician come Monday, methinks 
Animistic
Titanium Teammate
I think you're being a bit hard on yourself, seems you read the words fine, it was the comprehension that was a miss. May I suggest a cognitive psychologist? 
In all seriousness though, I think you're still right that the precipitate is likely sodium acetate. If it were dmt the shellite would take it up, it came from the shellite after all.
@Upnorth Do you still have the original purpley black basic soup?
In all seriousness though, I think you're still right that the precipitate is likely sodium acetate. If it were dmt the shellite would take it up, it came from the shellite after all.
@Upnorth Do you still have the original purpley black basic soup?
I dunno, which one would you say might be cheaper? Is Gag Halfrunt still practising?I think you're being a bit hard on yourself, seems you read the words fine, it was the comprehension that was a miss. May I suggest a cognitive psychologist?
This is what comes of posting while trying to fry a pancake and being in a hurry to get out of the door.
There's still a possibility that something has come through on the first shellite pull which has subsequently rendered insoluble by the A/B cycle, so I wouldn't bet my house on it being sodium acetate, maybe just my car.
SunshineMaker
May we never go to hell, but always be on our way.
I'm just seeing this conversation. We were in the same situation it sounds like, I ended up putting my first pull in the freezer for 24 hours and collected very little. My second pull was more yellow and I put that one in a jar to be refrigerated for 12-18 hours then transfered into a baking dish and put that in the freezer at half the max temp for 12 hours and then max temp for 3 days if I'm remembering correctly. Every few hours I would gently rock it back and forth for a few rotations. The slow drop in temp, agitation, and duration seemed to help immensely on my first ex ever. Alot learned , alot to learn.
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Thanks for all the replies, been busy with work and haven't been on here.
Unfortunately the lid broke on my 2l bottle so I dumped it. Going to make up a half size (50g root bark) on weekend and see if I have more luck with xylene pull. I did try suck up all the white stuff from bottom and put in a seperate jar with some warm naphtha and I'm pretty certain it isn't dmt as none of it went into the naphtha.
If the white crystals are sodium acetate they'd be water soluble. Not that this would constitute a positive identification, but it would be one more step towards working out what they could be, if "not DMT" proved to be insufficient an answer for you.
It looks like plant fats/matter that have been brought across with your shellite into the vinegar wash to me, common when backsalting Acacia, havent seen this much before but 
If it were me I'd just do some pulls on the solution as it is and pay attention to what happens to it.
If it were me I'd just do some pulls on the solution as it is and pay attention to what happens to it.
Thanks guys I currently have a new attempt at the basic soup stage. Going to pull with xylene then transfer it to naphtha on clean up if all goes well.
One thing I'm not too sure about with freeze precip is that I'm in a high humidity area so when I pull glass from freezer it will immediately make a condensation/frost layer on inside of glass tray. Will this cause issues on that step? And is there another option such as full evap to avoid this issue?
One thing I'm not too sure about with freeze precip is that I'm in a high humidity area so when I pull glass from freezer it will immediately make a condensation/frost layer on inside of glass tray. Will this cause issues on that step? And is there another option such as full evap to avoid this issue?
I hate the humidity I'm Australia.
Only way I've found to slightly mitigate this is.....
Pour off solvent, replace lid and back in the freezer upside down.
Wait another hour let residual solvent run off the crystals.
Remove from freezer and keep upside down with the lid on.
When almost at room temperature you can remove the lid and put dish Infront of a fan.
Inevitably you may still suffer from condensation depending on what the day is like but this method certainly helps.
Things like airconditioning/dehumidifier will make your life easier also.
Only way I've found to slightly mitigate this is.....
Pour off solvent, replace lid and back in the freezer upside down.
Wait another hour let residual solvent run off the crystals.
Remove from freezer and keep upside down with the lid on.
When almost at room temperature you can remove the lid and put dish Infront of a fan.
Inevitably you may still suffer from condensation depending on what the day is like but this method certainly helps.
Things like airconditioning/dehumidifier will make your life easier also.
I'd expect 50g of lye to be highly soluble in 200mL of water. It is very water soluble so I doubt that it is undissolved lye.
Like @Transform said it could be a precipitate that is insoluble in shellite, however in my experience with Acuminata and double A/B extraction the solution is pretty clear after final extraction with fresh solvent. Since your solution is probably cool by now, you could try pulling with something like xylene to see if it pulls your solid. If you are trying to pull with shellite from a cool solution, its sort of hard to negate the temperature aspect of using shellite for a conclusive result. Xylene or another non selective solvent should help tell you if it is an alkaloid or undissolved base.
And finally... if you are using the shellite of today then good luck getting a solid. It has clearly changed in composition and works very poorly for crystallization. Are there moisture beads left on top of a film of goo? If so, then I think it's likely a solvent issue. It is common with acuminata to get a film of oil.. it is still super clean DMT most of the time and you can follow the usual dosages.
Re: condensation, try putting some porous paper (like commercial oil filters) on top of your dish as a lid followed by cling film.. I've recently found oil filters really good for absorbing condensation from moisture in the external environment - any porous paper will help absorb water from humidity. I've found this particularly useful for evapping DCM which is subject to absorbing water.. unelss your paper is dripping wet it certainly shouldn't drip back down into your NP solvent.
But in Australia if you are using Bunnings shellite.. then I think that is the likely culprit behind the moisture in your extracts. The balance of hydrocarbons seems to have been changed in a way that invites water into your extract. Maybe someone could better explain why the change in hydrocarbon composition in naptha/shellite could lead to more moisture absorbtion.. that is, if at all. @Transform?
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Current best guess on the powdery precipitate is sodium acetate, forced out of solution by excess lye (maybe).
That's a really useful tip! Have you ever consider pre-drying the paper, say, at 110°C? Or would that be superfluous?
This really sounds as though there has been some kind of alcohol or other hydrophilic substance added to the mixture. IIRC, @benzyme looked into this when a similar situation arose in the USA and maybe detected the presence of PEG derivatives (recollection's a bit hazy on this one).
Thanks will give it a go. Ran out of time to finish today so have it sitting in acidic solution ready to pull xylene out, basify and add naphtha. Xylene came out more opaque than the naphtha did, naphtha came out yellow but clear. Feeling a bit hopeful it works this time.
So, you're defatting with xylene and pulling with naphtha? Or why is the xylene sat with an acidic solution?
This strikes me as a bit unusual. The DMT only starts coming out after you've added the base, right?
Just an update for all the guys who helped. I did the xylene extraction the transferred to shellite before freeze precip (flipping the tray while still on freezer, then turned freezer to +2 degrees Celsius and let it slowly warm up over a few hours). Ended up with 100mg of nice fluffy white crystals. Only did 2 pulls to see if I would be successful or not, so still have potential to get more out of it.
Thanks for all the help, couldn't have done it without all the guidence.
Thanks for all the help, couldn't have done it without all the guidence.
Ah, gotcha - you were pulling back out of the xylene. (I'm still pre my breakfast coffee and working on this hard puzzle - 2+2=… hmmm…
)Glad to hear it's worked out for you
So basically I used xylene in the basic soup with the acacia grounds, pulled xylene out into a jar, made a new mix with just water/vinegar, xylene. Mix the new mix around for a while to pull the DMT from the xylene into the acidic water, pull xylene out, add lye/water, add shellite and pull dmt from the new solution same way I did with the xylene/basic soup.