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First Extraction - Fail?

Migrated topic.
You've done your homework... it looks as though you are well-prepared to carry out the extraction. It seems like your giving ample time between each step. I don't know how much that will increase the yield; at least 0.50%-0.75% of the weight in bark can be extracted in about 2 hours. Your tek is fine; keeping the naphtha warm at the time of separation will maximize DMT saturation, but you don't seem to have missed any other detail.

SWIM may try doing Noman's tek in 2-3 hours but will save the solution for 24 hours to do another pull and see if any more goods come out.

And if I could give myself advice for my first extraction, I'd tell myself not to worry about purity until the recrystallization step. It takes a lot of energy to keep the naphtha really clean during pulls, and if you want beeeg honkin' crystals then you'll need to Re-X anyway.

Otherwise, be careful and have fun.
 
Newfound_wonder said:
You've done your homework... it looks as though you are well-prepared to carry out the extraction. It seems like your giving ample time between each step. I don't know how much that will increase the yield; at least 0.50%-0.75% of the weight in bark can be extracted in about 2 hours. Your tek is fine; keeping the naphtha warm at the time of separation will maximize DMT saturation, but you don't seem to have missed any other detail.
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I did write that after adding the Naphtha, to leave in a warm area for 24 hours
Did you mean that the Naphtha should be warm when adding to the H20/NaOH?
Or that after i separate it i should keep the Naphtha warm?

Its good to know i can extract,

And if I could give myself advice for my first extraction, I'd tell myself not to worry about purity until the recrystallization step. It takes a lot of energy to keep the naphtha really clean during pulls, and if you want beeeg honkin' crystals then you'll need to Re-X anyway.
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I'm very much looking forward to recrystallization & taking my time over the process :d

I'm wondering how slow to slow evap during re-X, can i leave the jar totally sealed & watch crystals grow?
Does that need more Naphtha in the jar? As you saw i'm only using just enough to redissolve the DMT...
 
Or that after i separate it i should keep the Naphtha warm?
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I'm saying you'll want the naphtha to be as warm as possible when you siphon it into the collection jar. Phrased differently, you should keep the naphtha warm before you separate it and when you separate it. Although, if the naphtha is too hot it may pick up other alkaloids (nothing that can't be cleaned up). After you separate it, you can freeze it. Personally, SWIM would rather extract every bit of spice plus some extras as opposed to extracting only DMT but not getting it all.

The saturation of DMT in naphtha is proportional to the temperature of the naphtha. The warmer it is, the more spice it can hold, and more spice can precipitate out when it gets put in the freezer. A warm water bath might work better than a warm room. SWIM puts the jar in a pot and adds some hot water to the pot to warm the solution before siphoning the naphtha.

I'm wondering how slow to slow evap during re-X, can i leave the jar totally sealed & watch crystals grow?
Click to expand...

As slow as you are willing to go. SWIM uses a shot glass exposed to open air and it works fine; pics and weights may come soon. It takes time though; watching crystals grow would be about as exciting as watching a pond freeze, but it's definitely fun to check up on it each day. Maybe taking a picture each day and making a still frame movie could help bring the crystal-growing process to life. Sealing it would definitely slow it down, but I don't know whether or not you need to have at least a little ventilation.

Who knows, maybe within a few days/weeks you'll be sharing crystal-growing advice with us.
 
Newfound_wonder said:
I'm saying you'll want the naphtha to be as warm as possible when you siphon it into the collection jar. Phrased differently, you should keep the naphtha warm before you separate it and when you separate it. Although, if the naphtha is too hot it may pick up other alkaloids (nothing that can't be cleaned up). After you separate it, you can freeze it. Personally, SWIM would rather extract every bit of spice plus some extras as opposed to extracting only DMT but not getting it all.

The saturation of DMT in naphtha is proportional to the temperature of the naphtha. The warmer it is, the more spice it can hold, and more spice can precipitate out when it gets put in the freezer. A warm water bath might work better than a warm room. SWIM puts the jar in a pot and adds some hot water to the pot to warm the solution before siphoning the naphtha.
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Cool, i don't mind getting yellowish crystals the first time, as then i can put a bit aside & compare to the white crystal later on, and im sure it'll make the re-X/purification enjoyably challenging

For people who have a lot around it must be tempting to re-X and just see what kinda size crystals you can make

I'll be sure to share some pics...
 
Got a few tips for your next one - so it goes quicker and smoother.

Chronic said:
DMT Tek:

Fill 5ltr Jug with 3.5ltr H20
Add 250g NaOH (caustic soda) into the H20 over ten minutes
Allow water time to cool & clear

Add 250g powdered Mimosa Hostilis Root Bark into the H20/NaOH solution
Place lid back on & swirl/roll contents until mixed together
Allow 24 hours for solution to break down cell walls & release DMT

Add 75-100ml Naphtha to solution (ronoson) & place jar in a warm area for 24 hours
(also add himalayan salt to aid in separation)
Ocassionally swirl, roll, turn upside down (don't shake) to mix contents
Ater 24 hours the Naphtha should have separated

Remove saturated Naphtha (w/ needle turkey baster) into 500ml jar
Allow just over half the Naphtha to evaporate (or until the Naphtha turns cloudy)
Put jar into the freezer for 72 hours allowing all the DMT to precipitate out (wrap in cling film)
Remove jar from freezer & gently pour off Naphtha back into the H20/NaOH/MHRB solution
Do this while the jar is still cold otherwise Naphtha may redissolve some crystals

Allow jar to sit at room temp & any remaining Naphtha to completely evaporate
Then scrape crystals
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I would suggest not letting the water cool - if you add the mimosa while the solution is very warm - the breakdown of cells takes a lot less time, which leads me to my next point - after adding the mimosa you don't need to wait more than 2 hours - I usually wait 1-1.5 - otherwise, again the whole solution gets cold, making seperation take longer when you add the solvent.

And lastly - Unless it's your 3rd and 4th pulls - I wouldn't let the naptha sit in the solution to seperate for more than an hour really, it usually only takes about 30-60 minutes to seperate.

I've found if you allow it to sit this long each step of the way - when you're doing your 3rd and/or 4th pulls, it's a real bitch to clean up as the solvent drags out A LOT of oils and fats.

Would like to know how things go though - it's seriously fun to do when you produce some nice crystals - my favourite one I have sitting on my shelf on a crystal slice. <3
 
Thanks for the tips, i'll make sure to add your updates to my tek :)

I was just wondering, is the freeze precip necessary if im reXing anyway?
 
Okay, so i mixed the H20/NaOH/MHRB, put it on a heater for 1 & 1/2 hours to keep it warm, then i emptied a can of newport lighter fluid (100ml) into a beaker & also brought a pan of water to the boil, as soon as it boiled i turned off the heat, added the beaker of Naphtha into the water & let it sit for a few minutes, i then added the hot Naphtha into the H20/NaOH/MHRB solution, agitated & let it separate 3 times, then i shall turkey baster off the Naphtha into a litre jar on the third time it separates, going to do 3 pulls (each 100ml) all into the same jar, then evap until it goes cloudy, then i will freeze precip :)

For some reason i felt to do hot pulls to make sure i get it all in 3 pulls, then i can clean it all up later on...
 
Remember to keep the mimosa soup till you have final yields. You might want to do a few more smaller pulls later on.

Otherwise all looks good man, looking forward to the pics:)
 
Chronic said:
Put jar into the freezer for 72 hours allowing all the DMT to precipitate out (wrap in cling film)
Remove jar from freezer & gently pour off Naphtha back into the H20/NaOH/MHRB solution
Do this while the jar is still cold otherwise Naphtha may redissolve some crystals
Click to expand...

After pouring the cold naptha off the precipitated crystals, I like to put the jar back in the freer but up side down just to make sure all the solvent has dripped off.

I then take it back out and let it evaporate further with the jar upside down, tilted up at one side to allow ventilation. This makes sure that the condensation forming on the cold glass runs out of the jar and not onto the crystals.
 
Unfortunately 100ml pulls in a 5 litre jerry can is just too much of a thin layer of naphtha to easily turkey baster off, maybe i shoulda used a milk bottle which would be slimmer.

I added the full 300ml naphtha into the solution & left it overnight, going to give it 24 hours and take the layer off tonight into a beaker, then take the layer off again into the freeze precip jar, i wanted to make sure i get as much as possible in this big pull as i doubt i'm doing another, maybe one just to see if i get anything...i won't throw the solution away.

I also had to shake a bit to get the naphtha to mix then separate, just rolling the container the nahptha wouldn't mix in at all, this morning i have a darkish layer of naphtha ready for me to collect when i get home from work, i have a feeling it's gonna take a bit of cleaning up, but i'm up for it... it seems as if theres 2 layers of naphtha, a thin clear one & a darker one underneath, then the solution underneath that, hopefully i didn't mess it up by shaking too much, it seems i may have emulsion...
 
when working with 4l of base solution, swim recently did 500ml/150ml at a time in a specially made jug with a mechanical stirrer.

he found a great 500ml olive oil bottle with a very thin neck and decanted into that after each 2h of mechanical stirring, it syringed off very easily like this.

yeild is good and the reliability of automated mechanical stirring made him not bother with 3 small pulls, just 1 large 1h pull per 500ml

2h per 500ml = 8h processing time plus around an hour bumbling around.

i'll post pics of that and some other lab equipment i made to make life easier in another thread at some point
 
I ended up with emulsion so added more lye & it separated back out fine, id been heating it quite a bit so now the Naphtha looks very coloured...

The Naphtha i managed to take off looks red to the eye, and if you shine a light on it it's yellow, im expecting a waxy red/yellow goo from what i've read...

Im thinking getting it out the jar is going to be difficult, maybe i should just evap on a tray, scrape then re-X? Or will a freeze precip still make some white crystals?
 
You can always try both. That's one thing I've learned is that there are many ways to do things and sometimes trying both when you're stuck is a good learning experience.
 
Im evaping with the jar on a radiator before doing a freeze precip, ive also been swirling it & the red larva type stuff has dropped to the bottom leaving a more yellowish colour liquid, theres also white clouds beginning to swirl around in there, which is think is the DMT.

I like that the liquid started red as that surely means i got a lot of the DMT out, with excess...
 
That's weird. I've never seen red naptha before but apparently it's not uncommon.
I would think the white cloudy stuff couldn't be the DMT yet. If you just started evaping it should still be in solution. Maybe it's lye contamination.
Maybe I'm wrong too. Thats always a possible.
 
I probably got red Naphtha as i did hot pulls & also had the container on a heater all night, i didn't let it drop to room temp at all, i also shaked it alot & had to add more lye to get the layers to separate, i was actually aiming to have very coloured Naphtha to know i got alot of the DMT aswell.

I hope its not lye contamination that sounds horrible, i only see the white clouds when i heat it, and thats when the red separates & drops to the bottom of the jar, hopefully the re-X/freeze precip will clean it up
 
The Naphtha may have cloudy stuff floating in it & be very yellow with a couple red bits mixed in, but it STINKS of DMT after sitting at room temp all day long!

I LOVE that smell, i obviously won't smell it too much cause of the Naphtha but it must be very concentrated to be stinking of DMT more than it smells of Naphtha

I added an extra 100ml Naphtha, threw everything back in the jug, shook it up, and letting it all separate back out a few times on the heater, also added some lye as it looked like it emulsified a bit or was taking a long time to separate.

This will be the final attempt to get all the DMT, i'll be happy with what i can get from this as im only expecting to journey a few times anyway, looking forward to that lovely smell when its all done :d
 
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