Does concentration affect harmine and harmaline precipitation

[Spiralout]

In short, the answer is yes: if you pay close attention to your solution, the crystals should precipitate out quicker.


:thumb_up:

 

[BongQuixote]

In short, the answer is yes: if you pay close attention to your solution, the crystals should precipitate out quicker.


:thumb_up:

That's 5 minutes in the penalty box for excessive punning.

 

[downwardsfromzero]

Harmala alkaloids can be precipitated by gaseous diffusion of ammonia from ammonia solution into a separate container of harmala solution using a larger, sealed, outer container. I have tried this and it works, and although my ammonia was far stronger than 10% I don't think that matters too much. This is an easy way of overcoming the problem of sudsy ammonia.

I will provide a pictorial for this in the near future.

 

[Daaren]

Thx Jees for the info on Zinc salts.
I didnt use any lye, only sodium carbonate in the early stages of the the extraction.

I did the separation using ammonia.

And the transformation of harmaline to thh using zinc powder and vinegar.
I then filtered and precipitated the thh using ammonia only.

What would be the salt in this case?

I tried to filter the salts and continue to basify but it was practically impossible to vacuum filter.
To the point my tubing collapsed.

Just for the sake of the experiment i also reduced the leftover water of a manske and after a night of sitting in the fridge more alks crashed out and the water/vinegar on top was now clear.

This leads me to wonder if there would be an optimal ratio of the concentration in harmala alks of the mother liquor / salt used
To precipitate almost everything during the manske .

This is an information i've seen rarely discussed on this forum for the past 10 years that i have been crawling here everynow and then. There is rarely information about concentration or even volumes. Its often dissolve in "some" vinegar. Or add some vinegar to enough water to .... just giving examples here...

I FEel that in the past alot of my extractions might not have been as efficient as they could have been and i lost alot of material to it.


Very interesting that i could precipitate alks using ammonia diffusion.
Thx for the tip Downwardsfromzero.

Also do you wash ammonia precipitated alks? Or they are good like that?

 

[Jees]

...I did the separation using ammonia.
And the transformation of harmaline to thh using zinc powder and vinegar.
I then filtered and precipitated the thh using ammonia only.
What would be the salt in this case?...

Good question actually, this non chemist kitchen fidler with coffee filters doesn't know, over to the real chemists please: is it this one? Zinc ammonium acetate

 

[downwardsfromzero]

And the transformation of harmaline to thh using zinc powder and vinegar.
I then filtered and precipitated the thh using ammonia only.

What would be the salt in this case?

THH is precipitated with ammonia as a free base, not as a salt.

 

[Daaren]

Sorry for the confusion i should have quoted the previous post.

Downwardfromzero:

Jees was mentioning the gel like phase might be zinc salts and depending on the base used this would vary.
In my case since i used ammonia it could not be zinc carbonate or zinc hydroxide...

I will take a moment eventually to learn to propery use the forum.
And also take time to turn on the computer to write here.

Posting on a forum using an iphone is not always easy

 

[BongQuixote]

Just for the sake of the experiment i also reduced the leftover water of a manske and after a night of sitting in the fridge more alks crashed out and the water/vinegar on top was now clear.

This is good practice. I do the same, reduce about 30% and then add additional salt for a second round of manske (I manske 5 times, so 10 total). In the future I think I will combine all the manske waters and do a more aggressive reduction, so I don't have to do the second round more than once.

 

[downwardsfromzero]

Catching up on some old business...

I will provide a pictorial for this in the near future.

Promises, promises. Life happened, then my camera broke. Someday in the not too distant future I still hope to do this.

In my case since i used ammonia it could not be zinc carbonate or zinc hydroxide...

Sorry for the misunderstanding! With ammonia you will still see a zinc hydroxide precipitate, at least sometimes. Or perhaps a basic zinc acetate gel - it can get a bit complicated even with this seemingly simple selection of cations and anions.

How did it pan out in the end, Daaren?

 

[downwardsfromzero]

Adding the bicarb very cautiously should minimise the harmaline co-precipitation, surely?

Probably yes, with pH kept low, hopefully just harmine precipitates.

I'll take a look at the figures and consider what might be a more effective base for this separation. There must be a more effective way - or is it unavoidably a matter of repeated A/B cycles?

Would be great to find some specific base just for this separation. What about some very weakly basic salt?

Things have been looking promising with ammonia and phosphoric acid after a magnesium reduction. Magnesium ammonium phosphate crashes fromaround pH 5.5 and only takes harmine with it in a tail-end fraction at pH 6.2. Nothing comes down after that until ca. pH 8. This suggests to me that ammonium phosphate buffering might help when basing with ammonia, perhaps even without the involvement of magnesium.