Lost During First Extraction - help wanted

[its0x11]

Ok here's my update. I have decanted all of the solutions I had before. Now I have a 2L media bottle with 1600ml brown and yellow liquid, possible some suspended particles, it's not clear but has no settled sediment.

I have 2 flasks now with approximately 600ml each of sediment and the liquid I could not decant the first time without losing the sediments. This definitely has some particles suspended in it still and some separated sediments on the bottom. I'm putting it all back in the fridge to settle again tonight so I can attempt to decant more tomorrow after further separation.

So what is my next step here after decanting again? Is there anything I can do with the brown liquid or is it all waste product? Is there a way to essentially do more pulls from it to collect more harmalas or should I just toss it? Just a little bit confused still since now I'm not really in the middle of any specific Tek and more just doing the basic chemistry at this point to try and salvage whatever remains.

 

[its0x11]

Forgot to attach the pics.

 

[doubledog]

Sediment is what you want.
If your liquid is at or above pH 11 you can toss it after proper settling, it's waste.

 

[doubledog]

Just a little bit confused still since now I'm not really in the middle of any specific Tek and more just doing the basic chemistry at this point to try and salvage whatever remains.

Just be patient, everything is fine, you clearly have lot of freebase harmala at the bottom of the bottles.
Harmala extraction after boiling phase is 95% waiting time, only 5% or even less of active work.

 

[its0x11]

Just be patient, everything is fine, you clearly have lot of freebase harmala at the bottom of the bottles.
Harmala extraction after boiling phase is 95% waiting time, only 5% or even less of active work.

It's a little over 10 right now. I can add more sodium carbonate or some lye to go back over 11. I went a little bit lighter this time because last time it was over 12 and took too much vinegar to get back to 4, which is why I'm here now.

 

[Sakkadelic]

It's a little over 10 right now. I can add more sodium carbonate or some lye to go back over 11. I went a little bit lighter this time because last time it was over 12 and took too much vinegar to get back to 4, which is why I'm here now.

That is alright, I suggest you decant, collect and combine all precipitate and proceed. You can keep the liquids and add more base and see if more precipitate comes out.

 

[its0x11]

That is alright, I suggest you decant, collect and combine all precipitate and proceed. You can keep the liquids and add more base and see if more precipitate comes out.

Perfect, I really appreciate you guys taking the time to answer all of my questions on this. Hopefully I'll be able to give back to the community more than I take later. I'm more of a mushroom guy than anything so these extractions have been totally new territory for me.

 

[doubledog]

because last time it was over 12 and took too much vinegar to get back to 4, which is why I'm here now.

This is little bit strange, as vinegar should easily acidify leftover precipitate, even when there is still some alkaline liquid.

 

[its0x11]

This is little bit strange, as vinegar should easily acidify leftover precipitate, even when there is still some alkaline liquid.

Yep, I was testing PH as I was adding vinegar. I probably added way too much lye the first time. It took nearly a liter of vinegar to get it to a 9.

 

[Sakkadelic]

Yep, I was testing PH as I was adding vinegar. I probably added way too much lye the first time. It took nearly a liter of vinegar to get it to a 9.

Yes that's another important point, in rue extraction you only need enough base or acid to convert the alkaloids, it's not about braking down plant material like in bark extraction. Excess base and acid only complicates things.

and it doesn't have to be exact pH values either, I never measured pH. During basification, you can check by putting a drop of base at the side of the jar and observe if it produces precipitate once it hits the solution. During acidification once the color changes and the solution is fluorescent under uv light or sunlight it's enough.

 

[doubledog]

If your precipitated leftovers are too alkaline, just wash out lye by adding water. You can also use some other non diluted acid like citric.
Ofc it's better to not add too much lye.

 

[its0x11]

Yes that's another important point, in rue extraction you only need enough base or acid to convert the alkaloids, it's not about braking down plant material like in bark extraction. Excess base and acid only complicates things.

and it doesn't have to be exact pH values either, I never measured pH. During basification, you can check by putting a drop of base at the side of the jar and observe if it produces precipitate once it hits the solution. During acidification once the color changes and the solution is fluorescent under uv light or sunlight it's enough.

Thanks for that. So right now I have a PH of 9 on the liquid and sediments but they're all visibly florescent yellow.

 

[Sakkadelic]

Thanks for that. So right now I have a PH of 9 on the liquid and sediments but they're all visibly florescent yellow.

What are you using for measuring pH?
The salt fluorescence is typically blue-green.
It might be that there's still some alkaloids dissolved in solution. In any case, seperating the precipitate from the liquid and adding more base to the liquid at this point is still the best course of action imo.

 

[its0x11]

What are you using for measuring pH?
The salt fluorescence is typically blue-green.
It might be that there's still some alkaloids dissolved in solution. In any case, seperating the precipitate from the liquid and adding more base to the liquid at this point is still the best course of action imo.

I have a PH meter with the little bulb on the end, calibrate it in the 7.0, then the 4.0 then the 10.1 solutions and then test the liquid

 

[its0x11]

Ok, so here's where I'm at and what I'm about to do. I decanted the flasks with sediments into a single flask and now I have about 500ml of sediment and some basic liquid, probably less than 100ml of liquid at this point.

I have a very small amount of sediment in the bottom of the 2L bottle that I did not waste my time trying to separate. Not worth the effort it looks like. Pics in the thread here so you can see what I mean. A lot of effort to try and decant 1600ml of liquid for a few grams of sediment.

I now have the sediment flask, 1600ml of basic fluid with a small amount of settled sediment and 800ml of decanted basic liquid with some suspended particles.

I'm letting the 2 media bottles come up to room temp and will put them on the stir plate and add some lye. Once they cool back off, I'll put them back in fridge for another 24 hours or so and see what settles out. Then I'll post another update before combining sediments again and either washing or going back to acid.

More pics here with an external light source so you can see the liquid's florescent yellow better and one with the UV so you can see the blue lighting up as well on the basic liquids.

 

[its0x11]

Alright, finished adding lye to my decanted basic liquid and let it sit for a moment, it's already started to separate again, so I guess 10 wasn't high enough for some reason. It went from brown and highlighter yellow to a more creamy brown color and it's beginning to separate. Looks like I'm going to have a LOT of sediment.

 

[its0x11]

After an hour of settling, seems like that was for sure the correct move.

 

[doubledog]

Imo pH should be 4 when it is in acidic phase and 11 or above when it's basic.

 

[Sakkadelic]

Nice! That's looking good.

Once you decant and combine all sediments, give it a water wash, reacidify, filter, and you should be good to go. Either base again to obtain freebase or do manske for the HCl salt