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Removing impurities left by solvent Options
 
youareall
#1 Posted : 11/13/2016 11:24:54 PM
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Dear Nexians

A character in a piece of musical theatre I am planning to write has just sucessfully extracted 2.8g xtals from 500g mimosa using STB method.

However on first use, our protaganist had a wonderful time, however woke up very short of breath and felt like that for a umber of days. He then realised that he had totally forgotten and failed to do an evaporation test (yes what a plonker). On then doing so with some remaining unused solvent he found it to leave quite a considerable amount of oily residue on the glass, which a moth then landed in and died just to prove the point...

So, now our protaganist must clean up the product, as it is currently highly toxic and unsafe for consumption.

He discovered this post https://www.dmt-nexus.me...aspx?g=posts&t=58096 recommending FASA for the same purpose, and is in posession of clean acetone and fumaric acid, however he fails to understand how this would remove the impurities. If xtals and fumaric acid are combined in the acetone and fumarate crystals form, but then the acetone is evaporated, then surely he will be left with fumarate crystals still with the solvent residue which has proven not to evaporate. He then mixes fumarate crystals with sodium carbonate to form freebase again, and mixes with acetone, at which point the freebase dissolves into acetone but sodium carbonate will not. he then filters out sodium carbonate. But as the impurities that he wants to remove are oily and not solids, will they not also pass through the filter along with the acetone containing the freebase? Or perhaps he is missing something, does one pass the acetone containing fumarate salt in the first stage through a filter instead of evaporation? but in the case wouldn't the oily solvent impurities become stuck in the filter along with the salt?

So he is now thinking of doing a mini A/B instead, would this clean it up better? But thinking about this, he is also wondering how this would work - would the naptha pulls with pure solvent (he now has a solvent which passes the evap test with flying colours), not also pick up the impurities from the old solvent, as they are probably soluble in naptha?

Regarding the mini A/B, he thinks he understands how to do it, but is unsure regarding quantities of vinegar, lye, and naptha, and he is finding it difficult to find out.

He is also concerned that he has just had xtals sitting in coffee filters in an airtight box at room temp with just one little sachet of silica gel for about 2 months now and is prettty concerned that his product may already be quite diminished?

Many thanks for your help!!
 

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Madrus
#2 Posted : 11/14/2016 2:21:27 AM

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If anyone wants help reading this:

I have just successfully extracted 2.8g xtals from 500g mimosa using STB method.

However on first use, I had a wonderful time, however woke up very short of breath and felt like that for a number of days. I then realized that I'd totally forgotten and failed to do an evaporation test. Then doing so with some remaining unused solvent, I found it to leave quite a considerable amount of oily residue on the glass, which a moth then landed in and died just to prove the point...

So, now I must clean up the product, as it is currently highly toxic and unsafe for consumption.

I discovered this post https://www.dmt-nexus.me...aspx?g=posts&t=58096 recommending FASA for the same purpose, and I have clean acetone and fumaric acid, however I fail to understand how this would remove the impurities. If xtals and fumaric acid are combined in the acetone and fumarate crystals form, but then the acetone is evaporated, then surely I will be left with fumarate crystals still with the solvent residue which has proven not to evaporate. I then mix fumarate crystals with sodium carbonate to form freebase again, and mix with acetone, at which point the freebase dissolves into acetone but sodium carbonate will not. I then filter out sodium carbonate. But as the impurities that I want to remove are oily and not solids, will they not also pass through the filter along with the acetone containing the freebase? Or perhaps I am missing something, does one pass the acetone containing fumarate salt in the first stage through a filter instead of evaporation? but in that case wouldn't the oily solvent impurities become stuck in the filter along with the salt?

So I am now thinking of doing a mini A/B instead, would this clean it up better? But thinking about this, I'm also wondering how this would work - would the naptha pulls with pure solvent (I now have a solvent which passes the evap test with flying colours), not also pick up the impurities from the old solvent, as they are probably soluble in naptha?

Regarding the mini A/B, I think I understand how to do it, but I'm unsure regarding quantities of vinegar, lye, and naptha, and I'm finding it difficult to find out.

I'm also concerned that I have just had xtals sitting in coffee filters in an airtight box at room temp with just one little sachet of silica gel for about 2 months now and I'm pretty concerned that my product may already be quite diminished?

Many thanks for your help!!
 
fathomlessness
#3 Posted : 11/14/2016 5:40:15 AM

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youareall wrote:

and is in posession of clean acetone and fumaric acid, however he fails to understand how this would remove the impurities.


What happends is that the DMT-fumarate precipitates out of the acetone... then you pour off the excess acetone which contains all the impurities.

After that you can also wash the DMT-fumarate in more acetone (if your paranoid). I tend to use excess fumaric acid in the beginning just to make sure I have all the dmt which the recomended amount is 309mg fumaric acid per 1g of DMT. I then use water to dissolve the DMT fumarate and pour the water off leaving unreacted fumaric acid behind, I do this a few times to make sure I have all the DMT-fumarate (I can tell because my DMT'fumarate is normally colored so I can tell be the water color when it is all gone).

Then you can either take your dried crystals and dump them in a base like your sodium carb and either dry it out and acetone the fresh crystals off OR (if you don't want to wait for water to dry which takes ages) then you can do a mini-A/B like u suggest and just pull with naphtha or whatever solvent you like.

Keep in mind though that fumaric acid wont react with DMT-n-oxide so that will be left behind. If you want to convert it you can use this tek https://wiki.dmt-nexus.m..._N-Oxide_to_Freebase_DMT

It is up to you whether you want to use excess fumaric acid and use water to dissolve the DMT-fumarate like I do or whether you want to stick to the standard ratios of 309-1g. Either way you MUST pour off the acetone in the begining after your DMT-fumarate has been born, THAT is where the impurities lie.

After all that I bet your naphtha was fine Laughing
 
downwardsfromzero
#4 Posted : 11/14/2016 8:04:09 PM

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Possible moral of story:

Freeze precip is better than evap (and always check your naphtha beforehand)~!


Bear in mind for FASA it helps if your acetone is as dry as possible.

When basing, you can pull from strong sodium carbonate soup with isopropanol (IPA).


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n0thing
#5 Posted : 11/15/2016 5:07:02 AM

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downwardsfromzero wrote:

Freeze precip is better than evap (and always check your naphtha beforehand)~!


Not always. I like storing it as DMT-fumarate crystals and when I run out of my batch I just do a mini-A/B. Storing freebase can be messy as it likely turns to goo after few days to weeks at room temp.

Quote:
Bear in mind for FASA it helps if your acetone is as dry as possible.


Good point, otherwise the DMT-fumarate will go in to the water in the acetone. It really needs to be 100% acetone.

Quote:
When basing, you can pull from strong sodium carbonate soup with isopropanol (IPA).


Yes, make sure that you coffee grind the sodium carb crystals up as the IPA or Acetone won't come in to contact because the DMT will be stuck inside the sod carb crystals.

 
Nereus
#6 Posted : 11/16/2016 12:30:07 PM

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Maybe you could also try to adapt this tek if there's a need for further re-xing after your initial clean up steps.
 
youareall
#7 Posted : 11/19/2016 1:24:47 PM
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fathomlessness wrote:
What happends is that the DMT-fumarate precipitates out of the acetone... then you pour off the excess acetone which contains all the impurities.


OK, that does make sense actually, but how does one pour off the acetone? Do the fumarate crystals stick to the bottom of the jar as with naptha freeze precipitation? Becasue I am imagining that if one poured through a coffee filter, then potentially those oily impurities that SWIM is trying to remove could also be caught in the filter along with the crystals?

fathomlessness wrote:
Keep in mind though that fumaric acid wont react with DMT-n-oxide so that will be left behind. If you want to convert it you can use this tek https://wiki.dmt-nexus.m..._N-Oxide_to_Freebase_DMT


how much of the product could potentially be n-oxide so potentially how much could be lost by not doing this step? or is that a how long is a piece of string question? this tek starts with n-oxide not dissolved in acetone, i guess in swim's case he would just add vinegar to his acetone containing n-oxide for the first step, and the n-oxide would then migrate to the vinegar?

thanks for all your help!
 
youareall
#8 Posted : 11/26/2016 4:53:23 PM
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bump! still confused about how the acetone is actually poured off? will the crystals stick to the bottom? Becasue if they are floating in the acetone and SWIM runs through a coffee filter, wont the impurities be caught in the filter? thanks!
 
 
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