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Letting particles settle after acid cook, experiment showing DMT is sinking to the bottom with them? Options
 
Emptiness
#1 Posted : 1/24/2019 7:20:18 AM
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Can anyone with more chemistry knowledge than I please help me understand what is going on here?

I like to prevent emulsions. So, instead of the hassle of filtering all those fine particles after the strain of the acid cook, I wait a few days for everything to settle to the bottom. What usually follows is sediment that appears to be amalgamated with oils.

I did a small experiment where i siphoned off the main clearer water on top and then put fresh water on the thick particle/oil bottom layer and stirred it up, then filtered it and did a mini extraction on both.

It was evident that both contained DMT, the sediment extraction colored the naphtha very yellow instantly while the clearer extraction didn't.

I thought during the cook the DMT disperses EQUALLY in to the water where it stays. Is this not true? Is the DMT sticking itself to the oil?
 

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leratiomyces
#2 Posted : 1/24/2019 9:30:59 AM
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Did you carry out the experiment to its conclusion? That is, did you isolate solid dmt from the two different aqueous extracts?
Obviously it wouldn't be a good idea from to draw conclusions from the colour of an organic extract.

I'm interested in your results as I've often wondered how much dmt gets caught up in the sludge that settles at the bottom. It's assumed that not much gets caught up as one would expect dmt acetate to have excellent solubility in water.
 
DansMaTete
#3 Posted : 1/24/2019 11:07:02 AM

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IME, sediment after acid cook still contain a lot of DMT. That's why you need to keep them for the next steps (base&pull). Or you can cook them (the sediments) in fresh water and decant again but you have to do it many time to keep a nice final yield.
I never understood this fear of emulsion, i shake like crazy and never had a bad emulsion with a MHRB acide/base extraction.

« I love the smell of boiling MHRB in the morning »
 
RoundAbout
#4 Posted : 1/24/2019 6:27:58 PM

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leratiomyces
#5 Posted : 1/24/2019 8:58:08 PM
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RoundAbout wrote:


Yeah, but only partially related, as adding egg whites is adding another variable. I big variable I would say.
 
RoundAbout
#6 Posted : 1/24/2019 9:35:53 PM

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leratiomyces wrote:
Yeah, but only partially related, as adding egg whites is adding another variable. I big variable I would say.


Yes, adding egg whites is a variable that could remove DMT. However a large portion of the DMT is held by the solids/oil(? ACRB?) after egg filtering, so that part is pretty directly comparable assuming this is MHRB or ACRB. What DMT-containing material is being used here anyways?

I am also wondering how was it evident that the solids contain DMT. Naphtha turning yellow doesn't indicate DMT (i.e. pure DMT dissolved in solvent is colourless) and doesn't indicate anything about the relative amounts.
 
Emptiness
#7 Posted : 2/2/2019 7:45:24 AM
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leratiomyces wrote:
Did you carry out the experiment to its conclusion? That is, did you isolate solid dmt from the two different aqueous extracts?
Obviously it wouldn't be a good idea from to draw conclusions from the colour of an organic extract.

I'm interested in your results as I've often wondered how much dmt gets caught up in the sludge that settles at the bottom. It's assumed that not much gets caught up as one would expect dmt acetate to have excellent solubility in water.


Yes, there was more DMT in the oily mixture, smelt way more like plastic too.

Do you think it has something to do with molecular weight? Falls through the water due to more atomic mass all the way to the bottom because of gravity?
 
Emptiness
#8 Posted : 2/2/2019 7:46:39 AM
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DansMaTete wrote:
IME, sediment after acid cook still contain a lot of DMT. That's why you need to keep them for the next steps (base&pull). Or you can cook them (the sediments) in fresh water and decant again but you have to do it many time to keep a nice final yield.
I never understood this fear of emulsion, i shake like crazy and never had a bad emulsion with a MHRB acide/base extraction.



For me its fine if i dont reduce. But i like to reduce more than 5x because it means i can save solvent and therefore money.

The more reduction there is, the less water and more fine particles and hence emulsion.
 
Emptiness
#9 Posted : 2/2/2019 7:47:25 AM
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RoundAbout wrote:


thanks, the bottom post in that thread says

Quote:
I've also noticed it is easier to decant the liquid without disturbing the sediment than to filter it. Then you reboil all your sediment, freeze and decant again if you want to get all the goods. Works with root barks and vine, but not rue.

Also if memory serves, refreezing and thawing the same brew a few times makes the solids get more and more clumpy and easier to remove.


also of note was the suggestion of this: https://en.wikipedia.org/wiki/Diatomaceous_earth
 
OwlMan
#10 Posted : 2/2/2019 11:00:10 PM

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How much acetic acid did you use? Did you check the pH? May be that it was not acid enough for all DMT to go into solution.
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leratiomyces
#11 Posted : 2/2/2019 11:40:06 PM
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Emptiness, can you provide more details please.
What's your starting material? And what was the mass of starting material?
What was the final mass of alkaloids obtained from the very first aqueous extract?
What was the final mass of alkaloids obtained from the aqueous extract of sediment?
What solvent are you using for extracting?
How are you isolating your alkaloids, freeze ppt or evaporation of solvent?

This info will help generate more plausible explanations for your observations.
 
Emptiness
#12 Posted : 2/3/2019 4:55:58 AM
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leratiomyces wrote:
Emptiness, can you provide more details please.
What's your starting material? And what was the mass of starting material?
What was the final mass of alkaloids obtained from the very first aqueous extract?
What was the final mass of alkaloids obtained from the aqueous extract of sediment?
What solvent are you using for extracting?
How are you isolating your alkaloids, freeze ppt or evaporation of solvent?

This info will help generate more plausible explanations for your observations.


Acacia, i didn't weigh it as it was clearly evident. The sediment extract had about 2/3s more. Was using naphtha at the time. Solvent evaporated completely.
 
Emptiness
#13 Posted : 2/3/2019 4:58:02 AM
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OwlMan wrote:
How much acetic acid did you use? Did you check the pH? May be that it was not acid enough for all DMT to go into solution.


Yes, from what i remember teks usually state 1 part vinegar to 7 parts water. I usually put 1/4 white vinegar. Ph never falls below 3 when i use vinegar, unlike hcl Confused
 
Mister Sunday
#14 Posted : 12/31/2019 11:16:40 AM
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Emptiness wrote:
OwlMan wrote:
How much acetic acid did you use? Did you check the pH? May be that it was not acid enough for all DMT to go into solution.


Yes, from what i remember teks usually state 1 part vinegar to 7 parts water. I usually put 1/4 white vinegar. Ph never falls below 3 when i use vinegar, unlike hcl Confused



Use just straight distilled white vinegar (5%).
 
 
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