Harmalas from rue

[isntme]

I'm currently testing teks for harmalas from rue. There are the following three teks I'm interested in; currently I'm doing the first two for 50g of seeds from the same batch each for a comparison if yields.

Tao (modified)
I decided to not grind the seeds, as this produced too much sludge, but only mash and freeze them after a first cook.
T1- cook the rue in acidic water for 1.5h
T2- mesh
T3- fill into doubled cotton undershirt sachet, close it
T4- cook for 1h
T5- freeze overnight - idea was to burst the cell walls
T6- cook 1h
- squeeze out, add only a bit of fresh acidic liquid to be able to work the sachet and squeeze (2x)
- add water - cook for next 'pull'
=> this gives me three fractions
T7- reduced to 360g | 180g | 140g (3 fractions)
T8- filter. filtration was super easy, even simpler than MHRB liquid. However even after filtration (1st fraction even twice), the liquid is not clear
T9- fridge decant / filter
T10- wash (water) to pH 7

Yields: 1.62g | 0,50g | 0,16g = 2.28g (4.56%) freebase before Manske


@Sakkadelic 's approach (if I understood correctly)
No grind, no initial filtration
S1- washed seeds (dust removal)
S2- cook for 3h at pH3 (started with 1l of water, reduced to just enough to cover seeds)
S3- decant (did not really squeeze out)
- add some acidic water, boil for 5 min
- decant and redo (in total 6 fractions)
added the first 5 fractions, let the 6th simmer for a few hours and sit over night (as a check)
S4- wash (water) to pH 7

Yields: 2.95g | 0.13g = 3.18g (6.36%)


@Brennendes Wasser 's approach
As Sakkadelic's approach but washing with water (not basified) until pH<8 to achieve the fastest way to usable freebase



Open questions
Q1) is a reducion of the tea volume necessary? I reduced the later pulls more, because there should be less alkaloids. The solubility of harmine / harmaline freebase in pH11 water is (afaik) 0.02g / 0.03g / 100ml; so this could be negligible. We use water washes anyways, so if to much would dissolve we wouldn't do this - right?

Q2) Sakkadelic washes with basified water (afaik), while BW uses normal water (to get rid of the base). My research concluded that harmalas in freebase form are comparably insoluble at pH7, but they may clump, which is not a problem I think. So why washing with basified water at all?

Q3) If we wash (with unbasified water) why then care for NaOH, it will be washed out anyways or not?

 

[isntme]

When letting settle after bringing to base, it stays at room temperature or would it go to the fridge?
Same question also for the manske step...

 

[doubledog]

Answer 1: Reduction is not necessary, you can base whole volume directly. Some losses are negligible, rue is cheap and has plenty of alkaloids. Reduction is recommended when extracting caapi ( very similar method as with rue, with slight modifications). I do not reduce rue tea at all.

A2: There is a possibility that harmaline could be washed away with lower ph / normal water. I would personally say that this would be preferable, as harmaline is quite unpleasant, but I believe that such washing is not happening at all or is minimal.

A3: Yes, hydroxid is washed away, but harm reduction is a priority here. It is important to emphasize risk of ingesting residual NaOH (or KOH). People make mistakes.

A4: for settling, it does not matter so much, but for manske you need to cool it. Manske step is based on harmala HCL's different solubility in hot and cold salty water.

 

[isntme]

Ok, thanks.
For manske cool is fridge 5°C or so right?
Or even freezer?

 

[doubledog]

Yes, fridge is ok.

 

[isntme]

Some images from the processing:
When adding the base, I waited for 2h and it looked as follows:

Then i tapped tha glasses hard on the the table, no 10 min later it looked as if everything had settled:

so this shortens the process massively!

The stuff at the bottom looks a bit colloidal (fluffy). There is much water in there, however it does not settle more even when waiting over night (as i did for one batch).
Washing in this stage costs much time and many washes (because there is so much liquid which can not be separated).
Therefore, I decided to build a simple centrifuge (I had the slants from mushroom breeding):



Before vs. after centrifuging for 20s


The liquid can then be decanted super easily and 4 washes is more than enough!

The water finally is clear / clean. However the harmalas are still browninsh:
See 'dried' and 'result'

 

[isntme]

Interesting yield result:
Tao (1.5h cooked, mashed, 1h cook, freeze, 1h cook and 2 additional fractions 1h cook each):
Yields: 1.62g | 0,50g | 0,16g = 2.28g (4.56%) freebase before Manske

Sakkadelic approach, only decanting (not even squeezing the seeds in my case), after initial 3h cook, further fraction only cooked for 5 min.:

Yields: 2.95g (fraction 1-5 combined) | 0.13g (6th fraction simmered for hours, let sit overnight) = 3.18g (6.36%)

So this is astonishing: just cooking and decanting the seeds, no filtering / fridge decanting has a higher yield.
One may argue that this is due to sludge, however the tea from seeds only was much more clear compared to the even twice filtered and fridge decanted stuff!
An the result is comparably brownish.
I think the filtering/decanting even though it was easy, not to much sludge did cost some yield.

=> Simplest approach is @Sakkadelic's: just boil the seeds, (decanting not squeezing hot seeds is enough), 5 or 6 short (5min) cooked extractions (after initial 3h cook) with just enough water to cover the seeds.

 

[isntme]

Preparing the manske step I have two related questions:
a)
I have acetic acid (25%) should I dilute this (how much) before resolving the freebase harmalas?

b)
In the Tao tek it is stated that one should have finally ~1L (per 100g seeds / ~6g freebase) with a final amount of 10-20g NaCl per 100ml. Do we really need to go for 1L?
When I calculated correctly I would strictly need about 1.12g of 25% acetic acid per g freebase to protonize everything.
Adding a factor 2.5 to be sure (2.8g 25% per g freebase) and + 1.5x as much water would mean I have
16.8g 25% + 25.2g = 42g diluted acetic acid which should dissolve my 6g freebase.

Now following Phlux's approach: preparing a saturated salt solution (~36g/100ml) and doubling the volume of the dissolved freebase, I would add another 42ml (giving me 18g/100ml salt) but only 82ml total volume, which is the minimum achievable and less than 1/10 of 1L.
I could add more water initially such that the total volume gets larger.

I use glass pans (as shown in the image above) which holds around 500ml at max and than has a liquidity height of 4-5cm.
The glass pan allows to collect stuff nicely as i can easily scrape it with a razor blade.
Would this provide enough height for the crystals? Or should I go for a tall and high container (not easy to collect crystals)?

 

[doubledog]

You can dilute freebase in quite small amount of slightly acidic water, but ime manske crystals need some space. 1 liter is maybe too much, but I would not go below 500ml for 6g of freebase.