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Noob freeze precipitation question

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Sandman013

Rising Star
Hello everyone, first of all i'd like to thanks all of you who helped with this process, i've been reading and reading a lot of posts in the past in order to study the perfect way to approach my first extraction, and it wouldn't be possible without this board

I've tried today my first extraction with Noman tek, which seemed easier and faster. I only have a couple of questions regarding the freeze precipitation:
1. should i just put in the pyrex all of the pulls i did, or separate pulls work best?
2. this is the most important one, for me. I'm kinda worried about contaminating my freezer (it's not only mine but also my girlfriends') and food in it, i thought about closing it with its lid, then wrapping it in plastic wrap and also putting all of it inside a plastic ziplock container. Should this be enough, or are there any other advice you think i should follow? I really don't wanna mess up my freezer or the food inside... :roll:

Thanks again!
 
downwardsfromzero said:
Excessively long contact with base could in principle lead to increased polymerisation of the DMT leading to a more deeply coloured, gooey product. The goo is also less soluble in naphtha, requiring more heating and maybe a heavier, less volatile naphtha should be used as a result.

If base soup has been standing for a fair while it may be worth pulling with another solvent such as toluene, xylene or limonene and recovering the product with an acidic back-extraction of some kind. A further alternative would be re-acidifying the soup in order to break down much of the alkaloid polymerisation and re-basifying as a sort of reset method for the extraction.

I was waiting for you :twisted:

At one point, I left a couple jars with 100g or bark in each sit in a base solution for a little over two months. I was able to get pure white DMT upon extracting, but it should be noted that I reheated the jars with the soup and used hot solvent which may have helped with decreased polymerization.

So listen to DF0 :)

One love
 
downwardsfromzero said:
Excessively long contact with base could in principle lead to increased polymerisation of the DMT leading to a more deeply coloured, gooey product. The goo is also less soluble in naphtha, requiring more heating and maybe a heavier, less volatile naphtha should be used as a result.

If base soup has been standing for a fair while it may be worth pulling with another solvent such as toluene, xylene or limonene and recovering the product with an acidic back-extraction of some kind. A further alternative would be re-acidifying the soup in order to break down much of the alkaloid polymerisation and re-basifying as a sort of reset method for the extraction.


Thanks for the exhausting response! I've actually not heated the naphta at all, but i guess the case you're mentioning is if the solution has been standing for a few weeks, not just 5-6 days
 
Sandman013 said:
downwardsfromzero said:
Excessively long contact with base could in principle lead to increased polymerisation of the DMT leading to a more deeply coloured, gooey product. The goo is also less soluble in naphtha, requiring more heating and maybe a heavier, less volatile naphtha should be used as a result.

If base soup has been standing for a fair while it may be worth pulling with another solvent such as toluene, xylene or limonene and recovering the product with an acidic back-extraction of some kind. A further alternative would be re-acidifying the soup in order to break down much of the alkaloid polymerisation and re-basifying as a sort of reset method for the extraction.


Thanks for the exhausting response! I've actually not heated the naphta at all, but i guess the case you're mentioning is if the solution has been standing for a few weeks, not just 5-6 days

Always heat your solvent (boil water, with the solvent away from the open and active heat source. Bring to a slight boil. TURN OFF THE HEAT SOURCE. Place the COVERED vessel of solvent in the water bath for about a minute. Pour into your extraction vessel and continue the process.) :D

One love
 
Voidmatrix said:
Sandman013 said:
I guess this must be done in order to extract more Product... I didn't do it because some said it wasn't necessary

I personally get way bigger yields when EVERYTHING is heated. I find it takes less pulls as well. Perhaps DF0 will be so kind as to give us the chemistry reason as to why. :)

One love
Naphtha is a fairly poor solvent for DMT - that's how it's so good for freeze precipitation. The flip side of this is that at higher temperatures the solubility increases in this particular case. The reasons why are probably beyond the scope of this thread.

Polymerised DMT is even less soluble in naphtha but it will dissolve in boiling heptane (98°C) and can be seen precipitating as an orange oil as the heptane cools. And this polymerisation can occur fairly rapidly under conditions of high pH and high ionic strength (more loosely put lots of dissolved salts, including the lye). Thus 5 or 6 days will be more than sufficient for some significant polymerisation to occur.

For a more exhaustive (and possibly exhausting:wink: ) look into these matters have a read of the Minimum polymer thread
 
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