Umm? Crap

[FiorSirtheoir]

Okay, being a little tired and not thinking properly I dissolved the hamalas I extracted in acidified water boiled it and didnt add salt. I then added the sodium bicarbonate to it. It didnt seem to precipitate properly. Can I go back and re acidify the water, boil it and add salt, or have I totally screwed up?

 

[soulfood]

nah, just reacidify it then salt as normal.

 

[FiorSirtheoir]

Salt is reacting to the sodium bicarbonate, it very fizzy.

 

[Ljosalfar]

You are better off converting the bicarbonate to carbonate. Or using NaOH.

 

[Enoon]

the acid may be reacting with the sodium-bicarb releasing CO2? in any case I get that when having added lots and lots of acid and then basing with Na2CO3 (sodium carbonate) and I have to add carbonate until it stops fizzing and only then will stuff start to precipitate.

But I agree using a stronger base is better, and personally I'm sold on lye - plus adding a bit of ethanol or IPA prior to basing with lye will get you pretty xtals it seem.

Anyway, happy experimenting. And remember this quote:
"I have not failed. I've just found 10,000 ways that won't work."
Thomas A. Edison

Cheers & love
Enoon

 

[FiorSirtheoir]

What about the acid solution being saturated with sodium? What effects will that have?

 

[Enoon]

with sodium? sodium chloride or sodium carbonate? not sure what the question is here.

adding sodium chloride to the acidic solution will let the harmalas drop out keeping the nasties in solution. this step is called Manske iirc. You only need it if you are extracting from rue; Caapi doesn't have any nasties worth separating like this.

adding sodium carbonate in excess to the acidic solution will make the harmalas precipitate. adding more than enough will do nothing. Any excess can and should be washed out during the washes you have to do anyway to remove the color. if you're worried about it being in your product just was one more time than you would normally using a large amount of water, stir well, let the goodies settle over a period of a few hours or a night and decant. It should be virtually free of Sodium Carbonate then. The same works for Lye and Lye gives more easily purified results IMO.

did this answer your question?

 

[FiorSirtheoir]

Enoon,

It did clear a few things up for me. My question, however, was this:

I neglected to add salt, late one night, but saturated the solution with sodium carbonate, it didnt seem to precipitate correctly. I had redissolved some hamalas I already had to refine it again. So, I re acidified the solution, which release the carbon, my question is what happens to the sodium? It stays dissolved in the solution correct? When you add sodium chloride, to a sodium saturated solution, the two( Na and Cl) will still separate correctly, to allow the alkaloids to bond to the chloride? It has been about 17 years since, a.p. chemistry, of which I don't recall much.

 

[Enoon]

Na2CO3 + some kind of acid => Na-acid salt + CO2 + H2O ... I would think
adding more sodium carbonate to that shouldn't hurt (you won't end up with sodium in your final product)

when you add sodium chloride to the solution, I think what happens is that the harmalas drop out because the water becomes saturated with the salt and just can't hold the other alkaloids anymore, I don't think they bind to the chloride. I could be wrong.

Either way you can acidify and rebase without worry. I would suggest using a stronger base than bicarbs though, unless you are trying to separate the alkaloids.