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sticky black tar from bottom of beaker after decanting Options
 
jibbs
#1 Posted : 6/19/2019 5:59:03 AM
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Hey guys,

So I am in the process of doing my second A/B using Vovin's tek using 100g MHRB. The first one went very well and so far this one is as well, except there is this one thing I did different and got an unexpected result. So after reducing the liquid from around 900ml to about 330ml I decided to do another fridge decanting because I had the time and wanted to see if any more particle would settle. To my surprise, the next day I didn't have the same kind of particles settled, but I did have a very thick, black, very sticky tar like substance that formed at the bottom of the beaker.

I don't know what this is, if it is garbage or if I should keep it and try and do something with it. I am doing the extraction on the liquid now, so I will see what I get out of it, but my concern is that something is wrong and that the DMT is actually in this tar substance. Could that be possible? Or is it more likely to be oils and fats and so stcky and thick because it was reduced? If it contains the spice, what do I do with it? I saved it just in case.

Has anybody else had this after a fridge decanting of a reduced MHRB liquid?



Cheers,

Jibbs
 

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blue.magic
#2 Posted : 6/19/2019 7:28:26 PM

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Technically it's very fine particles that make up the sludge.

I usually just decant the supernatant liquid, cover the sludge with fresh hot water, let it re-settle and decant again. Now the sludge contains little alkaloids so you can discard it.

A strong base (sodium or potassium hydroxide) will decompose the sludge to an extent. You can leave the sludge be in STB extraction, but I do A/B extraction and it tends to clog my separatory funnel so I remove it beforehand.
 
downwardsfromzero
#3 Posted : 6/19/2019 8:47:34 PM

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I think the sludge is to a large extent tannins. These are soluble in boiling water but precipitate very readily as an impenetrable sludge with minimal cooling. I found this out when trying to filter a hot acid boil from mimosa bark. It was clear (albeit very dark red) while poured out of the pan but turned thickly turbid in the filter and refused to pass through the filter paper. There's a chance that tannins could bind a fairly significant amount of alkaloid - thus BM's water wash is a prudent yield-enhancing step.

These tannins themselves are quite useful for treating certain skin diseases such as wet eczema. In case anyone wondered Big grin After all, that's what I use my mimosa bark for Very happy




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jibbs
#4 Posted : 6/20/2019 3:35:40 AM
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Thanks guys. I am melting it in hot water now and will decant and add to my mix. I didn't get to start my extraction last night, so I will finish this, add it and start basification and extraction. I will let you know how it goes!
 
blue.magic
#5 Posted : 6/20/2019 12:57:04 PM

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Yes tannins!

What I usually do is a quick hot gravity filtration (with a cheesecloth), then let the pot sit overnight and decant it the next day. The leftover sludge is what you are describing, sometimes I manage to squeeze it in a cheesecloth and it resembles a modelling clay Smile
 
jibbs
#6 Posted : 6/23/2019 8:47:00 AM
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Hey guys. I promised an update with the final product, so without further ado!

This is after the initial scraping plus one re-x with bestine / heptane. Yield was not as big as my first attempt using this tek and the initial scraping was more yellow than the first attempt as well. If cleaned up nicely after re-x though.

 
tripwire
#7 Posted : 9/9/2019 12:40:12 PM
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This sludge for me ended exploration of A/B routes and constrained me to focus on STB route exclusively. To my understanding, the advantage of the A/B route is the elimination of plant material from the initial aqueous solution. This can only be achieved with good yields by performing multiple boils and then reducing the combined boils to a manageable amount. But the solution will not reduce even by half without this sludge falling out. And this sludge does indeed contain actives. Without scope for even 50% reduction of initial combined boils, the viability of a clean A/B path ends right there. My recovery solution upon this discovery was to gently reduce everything to this thick tar (with lovely white streaks when cooled, the actives present clue), and then to reheat to 70 degrees and to keep at this temperature while adding naphtha and performing the pulls. I called it the Mordor method as the extraction was essentially performed at just below the temperature it would all blow up in my face. It was fantastic to see the naphtha cloud instantly it touched the cool glass of the pipette. As the naphtha pulls accumulated a yellow layer would form at bottom of beaker. After leaving to settle I decanted the clear warm naphtha away from the yellow layer. Is it possible dmt-oxide can be pulled by boiling naphtha? Anyway no evaporation of the clear fraction was necessary as totally saturated. I got the full expected yield from this melted black tar. I will hunt out a picture of the fully reduced tar with white streaks if anyone interested.

My question is, given that boiling the bark in acidic water will pull a phenomenal amount of this tar, is there another temperature or technique that will dissolve the alkaloids but leave the tar behind, so that reduction and filtering can be performed towards a clean A/B extraction?
 
 
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