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Freebase dark grey and solvent not rising to the top

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babagmn

Rising Star
Just had the above issue.

I did a warm acid extract with phosphoric acid 3 times with about 1 litre and then boiled it down and added noah to basefy it. But when I added the benzene the benzene is not separating out. It seems to be mixed in with the free base.

What went wrong? Did I add too much lye? The pH went from 2/3 to 13/14.

Is there anything I can do to rescue this?
 
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Thanks.
So should I add some water to this mixture to dilute it down?

I had another batch from the same mhrb and that seems fine. It's a very dark colour, almost black. I've not added any benzene to that though.
 
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As a quick update, I placed the bottle into a water bath around 60 Deg c and that section of the bottle the colour goes from a dull mat grey to a dark gloss black. There is a distinct color change and I can see the two separate layers.

Still can't see the clear benzene layer though.
 
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I've done this and there are three distinct layers. A dark murky layer on top, a blackish layer in the middle and a dull grey layer at the bottom.

There is certainly no clear layer of benzene.


What can I do next?

I did notice that there was a black shiny substrate burnt onto the glass from the bottle in the hot water. It looks the same as the burnt residue I got when grinding too fast in the grinder.

Really not sure what I have done wrong here. Would appreciate some expert help. Lots of thanks.
 
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babagmn said:
As a quick update, I placed the bottle into a water bath around 60 Deg c and that section of the bottle the colour goes from a dull mat grey to a dark gloss black. There is a distinct color change and I can see the two separate layers.

Still can't see the clear benzene layer though.
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Be careful with benzene, it’s banned in many places for a good reason. It’s highly toxic and linked to serious health issues. Make sure you’re following proper safety precautions, using protective gear, and work in a well-ventilated area.

Other than the addition of more water you can add salt to help with the separation. The top layer I suspect is going to be the benzene the middle the base soup and the bottom layer which I suspect is rather small could be some undissolved salts or courser fractures of your bark.
 
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Varallo said:
Be careful with benzene, it’s banned in many places for a good reason. It’s highly toxic and linked to serious health issues. Make sure you’re following proper safety precautions, using protective gear, and work in a well-ventilated area.

Other than the addition of more water you can add salt to help with the separation. The top layer I suspect is going to be the benzene the middle the base soup and the bottom layer which I suspect is rather small could be some undissolved salts or courser fractures of your bark.
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Ok. Thanks for that. What kind of salt can I use? Just normal nacl? And how much?
 
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On the eother batch I have a similar issue when I add the benzene. I get three layers. I get a clear benzene layer, a middle gooy layer that is light brown and almost cloud like. And then I have the bottom dark layer.

I have diluted that batch down with distilled water and the pH was clearly 12/13.

The benzene layer is separating out slowly.
 
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Wow. That seems to have done something.

The ones that had a cotton .Ike cloudy layer have now separated into a lower black layer and clear benzene on top.

I've added some salt the the one that had three layers without any clear benzene layer. Not used as much salt because that's a far bigger amount. I suppose I couple rake a small sample and add some more salt to that to see what happens. Might try that later.

Btw what is the salt doing? What's the chemistry going on?
 
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When salt (NaCl) is added to polar fase (water) it dissolves into Na⁺ and Cl⁻ ions, thereby increasing the ionic strength of the aqueous layer. This makes the water more polar and reduces its affinity for non-polar compounds, in your case benzene, forcing the non polar and polar to separate more strongly thereby solving emulsion problems and causing increased speed of separation between the layers.

By the way I am still rather concerned about you using benzene, could it be that you are mistaking benzene with benzine, as in lighter fluid. Benzene, a chemical known to cause leukemia and other diseases and is not something amateurs should be using when alternatives are so easily available.
 
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So I took a small sample from the one with no clear benzene layer and added salt to it. It seems to have done nothing to it.

Is there any way to rescue this soup. It may have the most amount of DMT it in.

I think I may have emulsified it somehow.
 
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Varallo said:
When salt (NaCl) is added to polar fase (water) it dissolves into Na⁺ and Cl⁻ ions, thereby increasing the ionic strength of the aqueous layer. This makes the water more polar and reduces its affinity for non-polar compounds, in your case benzene, forcing the non polar and polar to separate more strongly thereby solving emulsion problems and causing increased speed of separation between the layers.

By the way I am still rather concerned about you using benzene, could it be that you are mistaking benzene with benzine, as in lighter fluid. Benzene, a chemical known to cause leukemia and other diseases and is not something amateurs should be using when alternatives are so easily available.
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Thanks for that explanation.

I'm using what is known as cleaning benzine here in Germany, we buy it at the hardware store and can also buy something called wound benzine which is used for medical cleaning of wounds.

I leant about using that instead of naphtha form this forum. Does that make sense?
 
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Yes, it's called wash benzine and that translates to cleaning spirit.

So I'm still having issues with one of the extractions. Should I re acidify it using phosphoric acid and then rebasefy it? Will that help to solve my issue? I may well end up with a large amount of liquid to work with though. But at least I will not loose any of my spice.
 
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The salt has helped a little bit but I am still getting a very cloudy cotton like layer.

What about passing this all through a salt filter? That is fill up a coffee filter with salt and then pass the basefied and solvent mixture through that filter. Hopefully the liquid should just percolate through this.

Also what about using a vacuum chamber ? What effect will it have to place the mixture into a chamber and suck out the air to create a vacuum in it?
 
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Filtering will capture any freebase in the water too, so if you are going to filter then do so when the soup is acidic and dmt salts will be in solution.

However I think you have clear NPS as well now? If so then pipette that off the top first and freeze precipitate to see if there's any freebase in the NPS. Any emulsion layer is only an issue if it's in the majority and you've not pulled anything out with the NPS yet. Once you stop pulling product via the clear NPS layer then it's time to see if anything is captured in the emulsion.

Putting a container of soup in a vacuum chamber would do nothing worthwhile, you'll just boil off the NPS and then eventually the water.
 
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