Need help with a butchered extraction

[reun]

Hi all,

I recently ran an extraction process which I screwed up, so I'd like to do a bit of a post-mortem to make sure I learn from this and I might potentially still need to finish it off properly.

Here is the process that I followed:

1. Mix (until water was clear) 100 g of lye in 750 ml of distilled water, Do it in a few batches, then I let it sit for a few hours until the bottle reaches room temperature
2. Add 100 g of MHRB into the mixture and mix it periodically (2 minute swirls every 15 minutes) for about 3 hours
3. Add naphtha (evap test it first) and swirl it thoroughly. 4 hours later, when naphtha floated to the top, mix it again. Repeat it 4 times
4. Use a pipette to extract the top layer of naphtha and discard the rest (use a strainer to separate the bark from the liquid, throw the bark into the rubbish, while very very slowly, over 30 minutes or so, pour the liquid down the drain -- you are effectively using a powerful drain cleaner here. Important -- do that after handling the naphtha)
5. The naphtha should go into a Pyrex dish. Place a sheet of foil on top (that's a step I introduced later) and then close the lid, wrap it into cling wrap and place it into the freezer for 12-24 hours
6. Collect the naphtha from the freezer, pour it into another Pyrex dish, place a sheet of foil on top again, close the lid and place it into the freezer for another 12-24 hours
7. Return to the empty Pyrex dish -- it should contain DMT crystals, they should stick to the walls. Tilt the dish over a paper towel in a well-ventelated area and leave it to dry for 4-6 hours
8. Scrape the crystals with a razor blade, place them into an appropriate container and wash the dish
9. After doing 2-3 freezer rounds, place the remaining naphtha back into your original naphtha container -- you can reuse it for another extraction later

Alright, so I ran 2 extractions so far by following this process and so far both had problems.

Here is a quick overview of the problems from my first extraction:

• I used a flask with a foam top that also had a cork-type bottom on it, presumably designed to let the vapours out -- I did not initially realise the implications of that, but I guess I must have lost some naphtha and DMT with it
• I used a standard glass food container which I think did leak some naphtha through it -- I could smell it. I had to clean the freezer afterwards
• My 2nd freezer round yielded absolutely nothing
• I ended up extracting 500 mg, whereas I was expecting 1.5 g or so -- disappointing!

Here is my 2nd runthrough:

• I used the same dodgy flask, but I wrapped some foil on top of it and taped it up. I'm still not sure if it actually helped. Another important difference is that the first time I did all the naphtha mixes in one day, whereas the second time I spit it across 2 days, so there was more time for evaporation to occur, even if I tried to sorta stop it with the foil (not sure how important that is)
• After collecting naphtha into my container, I noticed that it was cloudy. I was not expecting that. I had to stop and do some digging to understand what the hell was going on. My research suggested that it was probably just saturated with DMT, so I placed the container into a bath of warm water and the cloudiness disappeared as my research suggested it should
• This time I used a Pyrex dish, I placed it into the freezer, but a few hours later, I was worried that it might still be leaking some naphtha vapours, so I checked the freezer and I could indeed smell some naphtha from the dish when I'd get up close to it. I freaked out a bit, I poured the naphtha into a Kilner glass jar, placed a foil wrap on top and then screwed the top part over it. But to be safe, I decided to take both the empty pyrex dish (it already began to form some DMT crystals) and the Kilner jar outside (the temperature was around 10 degrees Celsius) for the night because I just didn't want to worry about it while I sleep. The next morning, I decided to place both of them into the freezer for about 14 hours. In the evening, the Kilner jar had no crystals whatsoever while the pyrex dish had about the same amount of crystals it had when I took it after letting it sit for a few hours
• Overall, I ended up with about 100 mg of crystals, and then I returned the naphtha back into its original container. But then I started wondering if maybe it still had some DMT trapped in it that I just wasn't able to extract!

I have no idea what exactly failed, it could have been:

• A problematic flask
• checking whether cloudy naphtha is a problem by warming it
• Moving it into a different container after a few hours and then leaving it in 10 degrees for about 8 hours
• Perhaps DMT is still in that naphtha somehow, but I just couldn't extract it -- not sure what to do in this case!

Here is how I'm planning to iterate on it:

• Get a proper damn flask -- I'm getting a NULYLU lab flask with a screw on top -- I think it should hold naphtha, and I hope I won't need to resort to foil here
• Cloudy naphtha -- not a problem, I know that now, I will not screw around with it anymore
• Use a Pyrex dish with foil before closing the lid, then cling-wrap it and leave it in the freezer. I've also ordered some leak-proof media bottles made of super thick borosilicate with a GL45 screw, but I think they will be difficult to handle when it comes to scraping DMT off the walls, so I would love to avoid these
• If my next extraction round proves to be disappointing again, then I will start looking at alternative D-limonene based extractions like Q21Q21

I know this is a very long post now, so thank you very much if you've made it that far! I have a few questions for the readers:

• What do you see as the main failure points in the above?
• Do you feel like my proposed corrections for the future are sensible?
• Do you think that my naphtha could still be holding DMT? If so, what can I do with it if it did not want to freeze-precipitate out?
• Any other thoughts or suggestions?

Thank you again!

 

[fractals4life]

This is just a quick drive by post .. but what stands out to me is that you only add naphtha once then discard the bark soup.

You should be adding more naphtha after siphoning off the layer and repeating the swirling and separation several times until no more DMT comes out.

So after the first pulling off the top layer, do at least two more cycles of mixing in naphtha and extracting it. Ideally keep the pulls seperate and freeze precipitate each one to see how the amount of DMT gained from the soup is changing and stop the naphtha cycles only when the last one didn't yield enough to be worth the effort in your opinion.