Harmalas extract help

[Ludka]

I may have messed up my Harmalas extract. I was using a combination of 2 teks (might have been my first mistake), Tao of Rue and Harmalas Extraction and Separation Guide. It was after the first Manske that everything went south. I filtered the crystals out of the liquid and redissolved them in hot water.....only I added vinegar to the water as well. I saturated the mixture with salt, let it cool to room temp, then placed in the fridge to crystallize. Now the mixture looks like a yellow slushy.

Is there any saving this? I was thinking maybe base it again to neutralize the vinegar, but then the salt is still an issue. Any help would be greatly appreciated, thank you.

 

[Jagube]

Slush can result from Manske when too much salt is used or the cooling is too fast. I believe the slush is just small crystals as opposed to the nice long needles.

When I get slush, I filter it through a coffee filter, as decanting doesn't work so well. The slush that gets caught in the filter is as good as those long crystals you see in the pictures. Maybe a bit more contaminated with salt, but that's it. After dissolving in hot water and basing your freebase will be the same as if you started with long needles.

 

[Ludka]

Thank you for your reply. So the fact that I attempted to Manske with vinegar in the solution shouldn't matter then?

 

[Jagube]

Vinegar shouldn't do any harm here; it's just that it isn't necessary, because:

1. You're already dealing with harmalas in salt form (hydrochlorides in this case).
2. While Manske needs an acidic or neutral pH, harmala hydrochlorides are conveniently acidic in aqueous solutions due to the strong acidity of HCl.

Too much vinegar can add ions to the solution which may interfere with the precipitation. But I wouldn't know how much is too much.

 

[Ludka]

Thank you so much for your help! I was afraid I'd have to throw it out and start over.

 

[padawan]

A jar of yellow fluff is no drama. Good luck :thumb_up:

 

[Jees]

... I saturated the mixture with salt...

Try to lean toward 15 to 20 gr salt per 100ml of liquid. Then it all rests in the hands of your used concentration of alkaloids how it will precipitate from there.

Too concentrated:
* will get crystal forming (slush) even in very hot steaming liquid;
* you might not be able to decant any liquid at all if all went into slush.

Too low a concentration:
* even at room temperature there is little crystalization, needs a fridge and/or a lot of time to get it going well;
* possibly partly crystallization --> poor yield.
* if this happens, base the jar, filter out the extract, manske again in a lower volume.

 

[blue.magic]

Yes the "slush" is most probably harmalas crashed out too quickly.

You can boil the water redissolve the slush, then add little more water to decrease salt concentration and leave it to recrystallize. Or you can filter out the slush and repeat the process, but this may lead to losses and some salt gets trapped in the slush.

When my harmalas are very pure, only about 70 g/L salt is needed, but when impure, 150-200 g/L is needed.

In my experience, the crystals are usually bigger when vinegar is used as harmala acetates are more soluble then hydrochlorides.