Harmalas extraction-syrian rue (by SAKKADELIC)

[TGO]

Wow!

So as I mentioned earlier, I saved my original 5 boils and I am SO glad that I did! I ran through the process with 2 Manske on it. After basing for the final time, a TON of harmalas crashed out. It looks like another 10 or more grams! I couldn't believe my eyes, I was expecting a pitiful recovery of alkaloids but I was far off!

I am now estimating, I repeat, estimating d ) the total yield to be 20-25+ grams from 300g whole seeds! This is really amazing and a much more satisfying yield! See picture below:

You can see my blinds through the yellow tinted (yet clear, no visible particles floating) liquid along with the surprising (to me) amount of harmala FB. It is currently drying in a coffee filter. Total yield will be posted when fully dry!

In conclusion, if you are new to extracting harmalas and are using Sodium Carbonate as your base, I would recommend saving the liquid from your original boils and going through the whole process again. I couldn't believe the amount of alkaloids that were left over. I also recommend getting pH papers or a pH meter.

8)

 

[Jees]

:roll: :thumb_up:

Careful with estimating on sight though.

 

[TGO]

:roll: :thumb_up:

Careful with estimating on sight though.

Yes yes, of course! I was just really surprised and excited to see so much more crash out! I will let you guys know the actual total yield in a day or two when absolutely dry!

Also, I was reading about sodium carbonate contamination in the final product in this old thread. 69ron recommended taking the final product and doing this:

Now, what would be the best way to clean the product?

Trickster, the best solution at this point is to put the product in cold water with a little ice, and mix it for a few minutes. Then filter it until all the water and ice filter through. The sodium carbonate should dissolve and wash away. Harmine is insoluble in water, harmaline is very slightly soluble in cold water. Some loss of harmaline will be had, but no matter what you do, that’s going to happen. Even when you precipitate the alkaloids using salt water, some loss of harmaline occurs. Pretty much at every step in this process, there’s loss of harmaline.

Repeat if there's still some sodium carbonate taste left.

The are other options, but this is the easiest.

This is pretty much a water wash but as a final step...does anyone do this? Either way, what is everyone's thoughts on it?

 

[Jees]

To base:

* Do you add straight dry SodCarb powder to the pot with alks in?

* or are you making a separate pot with water and dissolve there the Sodium Carb til it is full watery, probably with some help of heat so that max saturation is guaranteed?
Bringing that pot to room temp again might crash out some sodcarb but this fallout you don't use. This fall out is good for re-use. You use the watery saturated layer to base.

I would use the second route to avoid SodCarb-powder in the end product that has never had the chance to dissolve fully and mimics FB. It only makes the scale happy.

 

[Jees]

With SodCarb in the end phase, I do 1 waterwash with fresh tap water. If pH of that water is 8 then I'm glad. Else one more wash.

Never measure pH of the wash water while the alks run around the meter/paper. Let settle some and the reading will drop then.

Just my take-on, glad to learn from others suggestions.


PS: with lye as a last base, that's a complete different game, then your're in for a wash week + weekend :surprised

 

[TGO]

To base:

* Do you add straight dry SodCarb powder to the pot with alks in?

* or are you making a separate pot with water and dissolve there the Sodium Carb til it is full watery, probably with some help of heat so that max saturation is guaranteed?
Bringing that pot to room temp again might crash out some sodcarb but this fallout you don't use. This fall out is good for re-use. You use the watery saturated layer to base.

I would use the second route to avoid SodCarb-powder in the end product that has never had the chance to dissolve fully and mimics FB. It only makes the scale happy.

I add dry Sodium carbonate to the acidic mixture, very slowly. I keep adding until it turns milky yellow and no longer changes color (roughly 50-100mg at a times...too much and it will overflow due to the reaction). This last time around (basing), I checked the pH with litmus paper and it was right around a pH of 10 (a little hard to discern the subtle color changes).

I think I'll consider using a saturated solution of sodium carbonate next time to see the comparable differences.

I don't think there is much, if any, sodium carbonate contamination because I added just enough base to get it where it needed to be. I was curious about water washing at the end and if anyone thought it would be a good idea to further purify the end product...

Edit: Ah, okay! I think at least one water wash is in order then!

 

[Jees]

... I checked the pH with litmus paper and it was right around a pH of 10 (a little hard to discern the subtle color changes)...

Yes those papers can be tricky. On pH 10 then 99.5% of harmine is FB, and 61% of harmaline.

For the first few A/B transitions I base with lye to 12 to get it all.
Only the very end basing done with sodium carb (IF i want fb at all for use) then the max is like 11.1 on some specs, but I got 11.55 before with good pH meter.

On 11.5 you have 99.9% harmine FB and 98% for harmaline (better than 61 :?: )

 

[ganesh]

PS: with lye as a last base, that's a complete different game, then your're in for a wash week + weekend :surprised

Surely that is if you previously over base, before washing. If you try to avoid that, and then simply wash the fb in a huge pot of water, then that should be sufficient for all intents and purposes, unless of course you need analytical grade purity, for gc-ms use.

 

[Jees]

Good point Ganesh (I go for pH 12 using lye, it's a reflex :lol: ), and there is something else bothering me in metering the PH after a water wash: if you take pH right after adding + swirling new water while the FB is still swimming around, the readout is quite high. Now if you let settle the FB and take pH of same water it can drop like 2 pH points.

* This wondered me if the FB hitting the pH probe is skewing the read out.

* Which of the 2 read outs it the one we should take serious?

Fuzz-ed :shock:

 

[ganesh]

Now if you let settle the FB and take pH of same water it can drop like 2 pH points.
* This wondered me if the FB hitting the pH probe is skewing the read out.

I guess that digital readings take time to adjust. Probably better to zero in between 'dips', with something of neutral ph for greater accuracy.

* Which of the 2 read outs it the one we should take serious?
Fuzz-ed :shock:

Untill you post another video, wearing blue gloves on your feet, i wouldn't let yourself take anything seriously! :lol:

 

[Jees]

LOL G :d

It has no relation to stabilizing the read out, I know of that issue. My new fancy meter has pronto reaction. I would ask people to meter both drifting and settled FB readings, if all meter no difference I must question my sanity

 

[ganesh]

. I would ask people to meter both drifting and settled FB readings, if all meter no difference I must question my sanity

'Forgetting about Jees newest video, wearing blue gloved feet in birkenstofs (as to not offend rue)':want: .... One might say 'JUST WASH THE SHIT OUTTA IT'?8)

You may say you tend to be 'anal' about purity, but thank your cotton socks that you havent gotten as sad as examining each and every individual seed for ensuring complete exhaustion of actives..YET! :lol:

 

[Sakkadelic]

if you take pH right after adding + swirling new water while the FB is still swimming around, the readout is quite high. Now if you let settle the FB and take pH of same water it can drop like 2 pH points.

* This wondered me if the FB hitting the pH probe is skewing the read out.

* Which of the 2 read outs it the one we should take serious?

Fuzz-ed Shocked

did u try measuring the PH after u decant the water, does it still measure high ?

 

[Jees]

Lol, OK please lets take this pH tidbit alleged wash-the-wormhole freebase fractalisation difference effect to a rest. I will check it out on my next rue process and if encountered again then I come back with bone hard core details that will blew ya outa whatever colored socks, only true Birkenstock adepts among you (only video proof is accepted) will be treated gently :twisted:

What did I start? :lol:

 

[TGO]

Alright folks, total yield (including 1 water wash at the end):

20.54g from 300g whole Syrian Rue seeds. Not too shabby, not to mention that will last me quite a while...:d

So 6% is definitely possible even with slightly larger amounts.

(Also, it seems to me that I must have not based the original boils anywhere near high enough on the first basing. Live and learn!)

Edit: Here is the pic of the FB in my designated harmala container!

 

[DoingKermit]

Man that looks nice! Well done :thumb_up:

 

[Jees]

...So 6% is definitely possible even with slightly larger amounts....

Yah man that is awesome. :thumb_up:

So you did 3 freeze/thaws;
7 Regular boils of 1 hour (0.5 liter + dash vinegar per 100 gr seeds), no microwaving;
7 times squeezing the seeds empty at end of each boil.
Collecting the 7 boils, evap volume to 1 liter, etc..

I guess the yield trick is narrowing down more and more around the item of the squeezing.
I think we're really done with just filtering the seeds, gotta hit them 8)

 

[ganesh]

I think we're really done with just filtering the seeds, gotta hit them 8)

Hey Jees.

Do you ever think maybe it's the squeezing of the seeds responsible for a good extract? Perhaps the shell is porous, it allows water to penetrate inside, but without squeezing they can's get out of the shell, which is so fine that it acts as a filter, which explains the no filter needed bit?

Perhaps the answer lies in just a couple of gentle boils, and soaking, but a focus on squeezing the goodness out, that boiling itself cannot do alone?

 

[Jees]

The successful numbers support that line of thought you bring up. :thumb_up:
Let's have a little 6%FB party

 

[DeeMenTalist]

Looking good TGO! :thumb_up: And thanks to the OP, will try this tek as soon as i get plenty amount of harmala.