[Logic Check] First time manske on Syrian Rue

[ooo0ooo]

Hi -

This is my first time doing an extraction of harmalas from Syrian Rue following the teks in the wiki. I'm now in the middle of the manske conversion to the salt and it's sitting in the fridge precipitating slowly after being left to cool overnight.

I just pulled it out and checked the jar under a black light and it is fluorescing a nice bright shade of green - both the precipitate at the bottom and all the rest of the liquid in the jar. (How cool is that?! 8))

No dramas, but just wondering -

1. If I got all the ratios right, would I be able to tell that the process was complete if the liquid portion stopped being fluorescent?

2. If after 24 hours or so, there's no more precipitate dropping, but the liquid portion still remains fluorescent, am I best off filtering and then re-heating the liquid with the addition of more salt or just basing it again and then repeating the manske?

Cheers!

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[Jox]

Hi oooOooo,

I think it is not going the right way for you, you shouldnt have any sedimentation on the bottom, this is plant material of no use. If you see pics of cristalisation they dont sediment but float in the solution like needles, I would discard the sedimentation and heat the solution a bit and add more salt to it and wait for the crystals.

Best
Jox

 

[ooo0ooo]

HI Jox -

Thanks for the reply. All good - definitely needle-like crystals that grew slowly bigger the longer I left it. Ended up staying the fridge for a week while I waited for some better filtration stuff to arrive.

When it got here, I checked under the black light again and it was much the same. Ended up pulling 9gms of the salt from the 200gms I started with. I've since re-based, filtered and that precipitate is drying.

I took the liquid from the manske stage, reduced and it's back in the fridge and dropping some more crystals again now. I'm going to keep fiddling with this and see if the liquid ever does stop fluorescing.

Interesting!

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[SnozzleBerry]

Sounds like you're doing just fine. I would disagree with Jox's assessment that you have not precipped mixed harmala hcl. Harmalas frequently precipitate at the bottom of containers, especially if there are a lot of them in solution.

1. If I got all the ratios right, would I be able to tell that the process was complete if the liquid portion stopped being fluorescent?

No, it will continue to fluoresce even after you've precipitated as much of the alkaloid content as possible.

2. If after 24 hours or so, there's no more precipitate dropping, but the liquid portion still remains fluorescent, am I best off filtering and then re-heating the liquid with the addition of more salt or just basing it again and then repeating the manske?

You are best off reducing. You can add more salt if you want to, but there's not really a need, as by reducing the volume you will be increasing the salt concentration. It's quite possible that you will even start to see salt falling out of the solution. Reducing, followed by re-chilling in the fridge/freezer should force anything truly desirable out of solution. As mentioned earlier, these alks may be less pure than the initial precipitates owing to greater salt contamination.

You can subsequently base your manske "waste water" once you've collected all of the alks that initially drop out, but this will yield very fatty alkaloids that are extremely time/labor intensive to clean and even with multiple cleanings, don't turn out anywhere as nice as the other alks. That said, we have analyzed these "waste water" precipitates and they are reasonably pure harmalas.

 

[ooo0ooo]

Thanks SnozzleBerry - I really appreciate the detailed reply and the benefit of your experience.

7.7gms of light tan out of 220gms source - 3.5% yield - that'd been sitting out in a hot shed for a year, (oops!). I'm happy with that result.

Cheers!

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[Jox]

SnoxxleBerry,

When dissolving the crystals in vinegar and rebasing to get free base harmalas is salt still present or not?

Thanks
jox

 

[SnozzleBerry]

When dissolving the crystals in vinegar and rebasing to get free base harmalas is salt still present or not?

So, with the major disclaimer being that I'm not a chemist, my understanding is no. When the NaCl is dissolved in vinegar, the Cl- ions bind to the harmala ions and the Na binds to the acetate ions. So, after you've collected your harmala hcl, unless you used an excess of salt, there shouldn't be much salt contamination, but there can be some. After redissolving, filtering and basing, I wouldn't think there should be any. I'm sure a chemist can correct the explanation if I'm mistaken