I did a harmala extraction a week ago , i salted my harmalas out then put in fresh water and sodium carb to wash it.
I percipitated my harmalas filtered and saved , more were still percipitating.

I decided to wash my 2 grams crude extract in the same solution.
I added and disolved it then procceded to add some more sodium carb
Nothing percipitated out.

I asked on the chat and was told to either acidify or basify then salt out again.

I added vinigar to my already sodium carb saturated solution with the harmalas still inside.
The solution fizzed,I added it little by little i then stirred and sat back , when i checked back on it it looked fine , but when i stirred it some more it fizzed again , and kept fizzing everytime i stirred it.

So nothing percipitated , i decided for anothe atempy , hoping it was acidic enough and added some salt , some disolved maybe i duno , theres lots of salt on the bottom so its saturated.

BUT NOTHING PERCIPITATED.

Does any one any any idea what i can do to retrieve my alakloids or what did i just do ?

I dont understand.. what do you mean, what solution? you had based and collected the extract.. Then you used the same base water where you just took it from and put the freebase harmalas?

As for all the fizzing, thats vinegar reacting with sodium carbonate and releasing CO2.. it does take a while, you can shake it many times and it will keep doing this, be patient.. what you can do is just let it stand and mix once in a while, and keep adding vinegar slowly after it stops fizzing or fizzes less.. this will make sure the whole thing is acidic.. then saturate with salt, mix very well, let in fridge overnight and hope that the harmalas will crash out

If adding sodium carbonate is what makes the base then yes i had a base i collected my harmalas from then proceeded with adding my freebase harmalas to clean and percipitate.

What volume of vinigar would i be able to add ?
- I wonder if 5% vinigar would do any harm to alkloids.

Also i feel as if it is already sooo saturated , would i be better off maybe splitting the volume and adding water or more plain vinigar to unsaturate it and acidify.

What happens to the sodium choloride when you try to re acidify ?

And what do you mean by hope it crashes out , why wouldnt it ?

have you tried cooling your solution in say a refridgerator for a few hours?

My solution has been sitting on a window shelf and is verry cold.

honestly I would rebasify the solution(add a lil more h20) and pull the harmalas with minimal naptha then evaporate. Their soluble in naptha freebase right?

I think you may have screwed the pooch by adding so much of this and that into it.

If you're using rue that mostly contains harmaline which is degraded by all solvents that aren't water as far as I know of.


Ok so you had freebase harmalas and you wanted to redesolve them to clean them further?

You only need the tiniest splash of vinegar to redesolve the alkaloids. I always did this in a pan, then kept adding salt until no more would desolve. If you can see a little bit of excess salt on the bottom of the pan, keep it on the heat for another ten minutes. If it desolves then add more salt.

Then just pour that into a jar and let it cool to room temperature, then put it in the freezer. As it's so salty it won't freeze, but everything should crash out nicely like that.

What do you mean so much this and that into it?
I added what was necessary and filtered during steps to remove anything that had not disolved.


Does this include acetone ?
This means the naptha is not plausable ?



I added a little more the just a splash , i hope this does not have any negative results.
-

Ok so i took my solution the other day and put it in a pan added some more vinigar and reheated it to near boiling, i then proceeded to add rock salt , not mutch disolved.
I left the rock salt inside just to make shure.
I let it cool and stuck in freezer for over a day and no percipitation.

Any Ideas on what i can do , it seems like ive tried everything , but there has to be a way of salvaging my harmalas.

As a last resort i want to evap the whole thing to a powder and redo everything.