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Harmalas extraction-syrian rue (by SAKKADELIC)

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Sakkadelic

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Donator
After reading some harmalas extraction teks on this site and understanding the basic ideas in them i tried to follow a similar method but with some modifications that i made and after repeating few times it turned out to be good. i hope for this method to be helpful for all and a good contribution to the site.

-why using this method?
This method is very easy to follow, it skips all the annoying filtering and produces high yields of clean harmalas.


-short description of the method:
soak whole syrian rue seeds with water and vinegar
freeze/thaw
boil vigorously in microwave
strain through a metallic strainer(or 100% cotton cloths) and press the liquid out of the seeds
mash with potato masher
repeat boiling/strain/press/mash 5-6x
combine strained liquid and basify with lye
settle and decant water
add water and vinegar, settle, filter, keep liquid
basify
water washes
add minimal amount of water and vinegar
manske
filter crystals, press water out with tissues, dry
collect HCl harmalas crystals
convert to freebase if FB is desired
dissolve crystals in hot water, basify
water washes
settle, decant, dry
collect FB harmalas


-resources needed:
whole syrian rue seeds(up to 100g more than that things get messy, larger volumes, hard to handle and strain...but can be done)
1L glass casserole or big wide jar(for microwave boils)
1L+ jar, 500ml jar, spare jars of different sizes that might come in handy
pure NaOH powder
distilled white vinegar
tap or distilled water
rock salt
microwave
freezer
potato masher
metallic strainer or 100% cotton clothes
large coffee filters
10ml syringe

step 1:acid boils (in this step the jars are very hot, use a towel when handling them)

-in a 500ml jar soak the whole seeds with 20ml vinegar and 230 ml warm water, stir and let them sit for 30 minutes, you could boil them a little if you want the idea is to soak them well and make sure they absorbed water. close the lid and put in freezer, once they are hard frozen remove the lid, put in microwave on thaw(on low). pour into the boiling glass container(casserole or wide jar) and put in microwave.
{
-boil 5 mins on high, let the casserole rest for 5 minutes stir then boil again for two minutes(if you are using a jar keep checking it might boil intensely and spill in the microwave if this is about to happen stop the microwave for few minutes then continue, placing a wooden spoon across the top of the jar will solve this problem and u can boil for longer but stay alert).
-let it rest and cool a bit then strain through the metallic strainer or the cotton cloth into the collecting jar or some temporary container(easier if you couldn't firmly fix the strainer/cloth to the mouth of the collecting jar then transfer later to the collecting jar), press/squeeze the seeds strongly until they are drained. if later the collecting jar was completely filled use one of the spare jars.
-put the seeds back into the casserole mash them slowly with the potato masher (be careful not to break the casserole sometimes there is small stones with the seeds) add 20ml vinegar and 230ml water.
}repeat this 5-6 times.


note: no need to follow procedure and volumes precisely, boil in enough water and vinegar strain and SQUEEZE the water out, achieve this the way that suits you.

-end of step 1:
you should end up with a dark brown/red tea in the collecting jar.
wait until it cools and start step 2, you can put it in the fridge but don't let it get really cold

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step 2:basifying
-prepare a strong solution of NaOH by dissolving around 50g of lye in 250ml water in one of the spare jars, first take all safety measurements before working with NaOH, slowly add NaOH powder to the water stir carefully until all powder is dissolved, this reaction is highly exothermic the jar will become very hot and the water might boil so be careful, this solution will be used throughout this extraction and probably in another one so store it properly if possible.
-when the tea is at room temperature, stir then using the syringe add the lye solution slowly and witness the beauty of this reaction, when the solution turns all milky stop adding lye, if there's still a distinct yellow tint in the cloudy solution add few more drops of lye until the tinge disappears.
-wait few hours until all the freebase has settled at the bottom, and pour slowly as much as possible of the liquid in the drainer be careful not to pour any of the precipitate along. i am impatient and don't have a lot of time usually so i just wait 2 hours max, there would be still some very fine FB floating around but it seems inconsiderable so i pour it, optimally wait 8 hours.

-end of step 2:
you should end up with a dark beige mud.

---------------------------------

step 3:removing impurities
-using the cleaned syringe add vinegar to the mud and stir until nothing is dissolving anymore, these are plant material sometimes they look similar to FB harmalas but don't add too much vinegar to dissolve them, they won't dissolve, so when the solution is not cloudy anymore and if you could measure PH and reached PH 4 stop adding vinegar.
-wait for the impurities to settle (1/2 hour is good), fix well a coffee filter on the jar and wet it with water, pour the solution slowly through the filter leaving the impurities to filter at the end so they don't clog the filter from the beginning, discard the impurities.

-end of step 3:
you should end up with a clearer brown to yellow liquid.


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step 4:re basifying and water washes
-stir and then using the cleaned syringe add the lye solution slowly until it turns all cloudy it will be more beautiful this time fill the rest of the jar with water, wait few hours for settling, decant water
-refill the jar with water, wait for settling and pour the water out this was a water wash, i usually do this until when i rub a drop of the water with my fingers it's no longer slippery(don't forget to wash your hands immediately), with each additional water wash the water will become clearer and clearer but the PH must not drop a lot so the freebase don't dissolves back into solution.

-end of step 4:
after decanting the last water wash you should end up with a clear beige to white mud


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step 5:manske and collecting the crystals
-transfer the mud to the 500 ml jar, using the cleaned syringe add slowly a minimal amount of warm 50-50 water-vinegar to the mud until it's completely dissolved.
-measure the volume of the solution you have or simply fill an identical jar with the same amount of water
-boil this water in microwave add rock salt and stir until all is dissolved(35g salt for every 100ml water will saturate the solution)
-add the salt saturated water through a filter to the harmalas acidic solution, screw the lid loosely and place the jar in a pot of freshly boiled water close the pot lid and let them sit undisturbed to cool of slowly for at least 12 hours.
-when the beautiful needles has crashed out, give the jar a little swirl so the crystals brake of the sides of the jar put them in the fridge for half an hour to settle and cool a little bit more, fix a coffee filter firmly(using a rubber) on the mouth of a jar and slowly pour first the water layer then the crystal rich layer through the filer, if while pouring the filter got filled stop for a minute until the water drips through it then continue, place the lid on the jar and leave it to drip the water.
-once the filter stops dripping water take it and fold it and fix it with clothespins or anything similar so the crystals are safe inside
-place the filter between 2 folded tissues on a dish, flip the filter and replace tissues every few minutes do it until no more water is coming out on the tissues, u can exert a little pressure on it with your hand to force more water out on the tissues, this will ensure that most of the salt contaminated water is out and you'll have a purer product
-dry the filter in front of a fan or using a hair drier, make sure that the filter is cracker dry before collecting the crystals (it will take around 15 mins using a hair drier).
-collect the crystals and store.

(sometimes when working with smaller amounts i proceed a little differently i calculate the amount of salt needed to saturate the volume of harmalas solution, boil in microwave and add a little bit less of the calculated amount of salt to it and stir until most is dissolved then filter the solution and continue normally, i get same results but i believe it's better when the harmalas solution is not saturated enough-with harmalas-).


-end of step 5:
you should end up with beautiful golden thin chips/foils(if using hair drier) of harmalas HCl crystals.(that's the best way i can describe them)

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step 6:freebase
-in a 500ml jar dissolve the crystals with a minimal amount of hot water, add lye drop by drop and swirl gently until the solution turn cloudy
-top the jar with water and rub a drop of the water in the jar between your fingers(wash hands immediately) if it's slippery then you need need to do more water washes, once it is not slippery anymore, dip the tip of your finger into the water then taste it, it should be tasteless, if it is sour or burns a bit then do more washes until is tasteless tasteless and feels like normal water.
-after the final wash let the jar sit until all freebase has settled at the bottom, decant very slowly as much as possible of the water, pour the mud into a narrow cup, wash the jar with few mls of water and into the cup. let it settle very well for many hours and with the syringe remove as much as possible of the water layer.
forget about using the syringe to remove the last bit of water, use a folded paper towel to slowly suck up most of the water, don't let the paper towel touch the freebase layer, picture describes it best.
-pour the mud in the cup into a wide dish and wash the cup with few mls of water and into the dish, dry it overnight in front of a fan make sure it's completely dry before scraping with a razor blade it will be very powdery when it's well dried

(right before complete drying if the freebase is scraped it will form a paste, if you dry this paste in oven on low setting you will get a solid peace like chalk that you can break into small stones of FB harmalas instead of the very fine powder, i like to do this bcz it's easier to handle and to smoke as it is through a pipe or bong, if you smoke a good amount of FB harmalas through a bong you will really get blown away, i wanted to write a post about the smoking experience of pure FB harmalas through bong experienced by me and 2 other friends but it's hard to describe this kind of effects, it's quite intense...)

-end of step 6:
you should end up with a clear beige to white freebase harmalas powder.

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this post was edited so sorry if any of the comments seem irrelevant.
images attached below are of different stages of the extraction and sorry for the rotated and not in order images.
 

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I pass all credits to the lab coats and the people carrying this site.
About "household": it sounds friendly but lye etc is to be taken carefully.
 
No need to use lye if you can get baking soda!

You can use the baking soda to precipitate harmine, then take some baking soda that you have baked in the oven at 400F for a few hours (sodium carbonate) and use that to precipitate harmaline.

You probably already know this Jees, just passing a friendly reminder along in the thread.
 
Agreed, I like this method. I am currently testing it out on 300g of whole seeds but I am substituting sodium carb for lye. Also I did regular acid boils (5x1h and squeezing in an old shirt) on the stove versus the microwave. Right now I am at the first basification with 1L of rue tea. Waiting for it to cool a bit before basing.

I :love: :love: :love: the idea of not having to filter so much! I plan on doing at least one filter during one (or more) acid stages. Thank you guys for putting out this useful information!

:thumb_up: :thumb_up:
 
May your endeavors be blessed :love:

When thinking lately about the workflow, I wondered if it might be beneficial to get the seeds more full of water before the first freezing act. So that the water in the seeds do a better freeze action. For this I thought maybe to do a first boil so the seeds can soak up max water. Then freeze/thaw.
 
I was thinking about the same thing jees but we are doing more than enough, my next objective is to minimize the time and make sure it works on larger scales maintaining 6% yields. I'm glad people are liking this method and i'm interested to know the yields u will get The Grateful One :)
 
Okay, so here we are so far and this is what has happened:

0. Freeze and thawed whole seeds 3 times

1. Boiled 300g whole seeds with approximately 1-1.5L of water and dash of vinegar for each 1 hour boil. 5 times. (did an extra two boils (total of 7x1 hour boils) on it just in case, haven't based the extra boils or anything yet).

2. Squeezed liquid out of seeds using an old white T-shirt after each boil. By the 7th boil, the liquid being squeezed was nearly completely clear, like water. The t-shirt also acted as a filter for each boil, obviously.

3. Reduced squeezed liquid down to 1L on stove. Allowed it to cool. Poured into 32oz "beaker" ...it is actually the glass part of a french press with all other parts removed...:lol: I actually ended up splitting it into two glass "beakers"

4.Based with sodium carbonate until the color stopped changing. Allowed to settle at room temp for a couple hours and then allowed to settle overnight in the fridge.

5.Carefully poured off the liquid. Kept the solids.

6. Boiled some water and vinegar and allowed it to cool for a couple minutes (approximately 2L...1L for each beaker). Poured this into the solids/mud. Allowed whatever goodies time to dissolve and stirred it thoroughly.

7.While the solution was still very hot I saturated each beaker with Salt. Stirred thoroughly. Allowed to cool at room temp for several hours and then in the fridge again overnight.

8.Carefully decanted the liquid and then filtered the solids through coffee filters to catch the goodies. I must note that the filtering at this stage went much faster than normal.

9. Redissolved the harmala salts into their respective beakers in approximately 1L of hot vinegar and water per beaker. Once dissolved and the color changed back to that beautiful deep dark red/brown, I decided to filter through a coffee filter. Kept liquids, discarded solids.

10. Based acidic solution with sodium carbonate again until the color stopped changing (mustard yellow). Allowed to cool and then placed in fridge to settle.

This is currently where I am in the process. I know it is not exactly how Sakkadelic wrote it up but I am mixing and matching things from different teks here and there. But it is basically the same concept. It is much easier with whole seeds. WAY LESS TIME CONSUMING FILTERING! That is the best part about it.

Now, I could recover my freebase and use as is but I think I will do at least one water wash seeing as I have not done one yet. I may also acidify and do another manske just to purify further. Then I'll convert it to freebase one last time and report the final yield.

The pic is showing where I am right now. The freebase harmalas are settling in the fridge. The dark brown sludge beaker on the far left is what was left after I based the original boiled tea again to see if anything was missed. The jug behind the yellow filled beakers is the remaining Rue tea (the last two "extra" boils) that I plan on going through this whole process with to see if anything remains. So no final yield yet but you can probably get an idea just by looking at this pic. These beakers are 32oz....seems to be a decent amount...not sure about 6 or 7% but then again I have only extracted Syrian Rue a handful of times so I am by no means, an expert! :d

*Got my camera working! Hooray!*
:)
 

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Keep up the good work 😉

I find the liquid above the FB to be very yellow, is it based enough with the sodium carbonate? At pH 10 you have 99.5% of the harmine in FB, yet 2/3 of the harmaline is still in water solution, just to give an idea. What is the pH in those pots please?

I'm not used to work with sodium carbonate, could be that too making the yellow.
 
Jees said:
I find the liquid above the FB to be very yellow
I think it could be the sodium carbonate because at this stage(assuming that it's been settling for enough time) even if the ph is low and the harmine/harmaline is still in the salt form the solution will look watery yellow not milky yellow.
the grateful one, thank u for ur work :) and at the end of step 6 did all the solids dissolve? If yes then using a shirt will help reducing 2 steps of the tek.
 
Sakkadelic said:
...(assuming that it's been settling for enough time)...
Yes that is important to know, TGO will tell us soon ;)

This is how my basings look like with lye till pH 12:
resource.ashx


I've always been a tad anal about having all the alks precipitated, and wondered if some lower yield reports are result of losing alks by not basing high enough.
 
ganesh said:
What about simply boiling seeds,ensuring they are filtered, then basing them once. Would that be good enough as a freebase to use, if one isn't overly fussy?
It would be an improvement over plain seeds or a tea thereof. It would still contain appreciable amounts of substances other than harmaline and harmine, for example vasicine and vasicinone. In some respects, these are interesting compounds in their own right. They can however cause uterine distress in females, potentially even provoke an abortion.
 
pitubo said:
vasicine and vasicinone. In some respects, these are interesting compounds in their own right. They can however cause uterine distress in females, potentially even provoke an abortion.

Yes, good point; Well done for pointing that out, but i'm a male, so i've no issues with the extra Alk's. Thing is i've read others saying these purification steps are good, but at cost of potency and full MAO inhibition per req'd dose. It's a case of balance.
 
Jees said:
Keep up the good work 😉

I find the liquid above the FB to be very yellow, is it based enough with the sodium carbonate? At pH 10 you have 99.5% of the harmine in FB, yet 2/3 of the harmaline is still in water solution, just to give an idea. What is the pH in those pots please?

I'm not used to work with sodium carbonate, could be that too making the yellow.

I'm not sure what the pH is because I do not own a pH meter...:oops: I think I'll order one today! Any tips on what brand to use would be much appreciated! It was indeed very yellow! You can't tell from the picture but it was more of clear yellow than milky yellow, as Sakkadelic mentioned.

When I took the picture the mix had been sitting in the fridge for about an hour. The harmalas settled very fast. I let it sit overnight again regardless. What is strange is that it slowly lost that bright yellow color and started turning back into that brownish red color. I added more sodium carb today when I got off work and now the mix is brown and settling just in case if I did not base it enough. Don't know if that color change is normal or not...?

Any other time I've used sodium carbonate the solution turns yellow upon basing and deep red/brown upon acidifying.

Sakkadelic said:
and at the end of step 6 did all the solids dissolve? If yes then using a shirt will help reducing 2 steps of the tek.

Yes, mostly. There were some impurities that settled, but not a lot which is why I went ahead and saturated with salt at that point. Then when I filtered during the next acidic stage, it went through coffee filters pretty easily with minimal impurities.

Like I mentioned above, the liquid above the FB harmalas was pretty clear except for the yellow tint. Hope this clears things up a bit!

EDIT: I can't see your picture for some reason, Jees! :p
 
ganesh said:
Thing is i've read others saying these purification steps are good, but at cost of potency and full MAO inhibition per req'd dose.
Are you referring to this recent post in particular? That is the only report that I have so far seen that claims this. It is not my personal experience. I see no mechanism for how the potency would drop, nor did the reported indicate any possible explanation. Based on my information, I wouldn't classify this as a tested and established fact, more as a single personal report.

IMHO you should simply perform the different purification stages yourself and try the results of different grades of purification for yourself. If you can find repeatable results, please report them here, so we can increase and refine our common body of knowledge.
 
The Grateful One said:
...What is strange is that it slowly lost that bright yellow color and started turning back into that brownish red color. I added more sodium carb today when I got off work and now the mix is brown and settling just in case if I did not base it enough. Don't know if that color change is normal or not...?
1 hour settling time is not enough, then there are still a lot of fines (FB) drifting in the water making the water yellow-ish. After those fines are also settled then you get the darker color because the bright fines are now all down. So it looks pretty normal what you describe.
Personally I keep repeating some A/B transits ( & filtering each acid state, finer filter each time) until the water above the settled FB is kinda clear (see pic below). Then I do my first manske. Just a habit of workflow.

The Grateful One said:
... I can't see your picture for some reason, Jees!...
You must have forgotten to pay your contributions? ;)
It does show on my screen, will attach here extra:
 

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pitubo said:
ganesh said:
Thing is i've read others saying these purification steps are good, but at cost of potency and full MAO inhibition per req'd dose.
Are you referring to this recent post in particular? That is the only report that I have so far seen that claims this. It is not my personal experience. I see no mechanism for how the potency would drop, nor did the reported indicate any possible explanation. Based on my information, I wouldn't classify this as a tested and established fact, more as a single personal report.

Ok, thanks for clarifying that.
 
I've never done more than 2 manskes, can't see the benefit for more, also because I do manske after several A/B's first that do the major cleanup.
 
Jees said:
The Grateful One said:
...What is strange is that it slowly lost that bright yellow color and started turning back into that brownish red color. I added more sodium carb today when I got off work and now the mix is brown and settling just in case if I did not base it enough. Don't know if that color change is normal or not...?
1 hour settling time is not enough, then there are still a lot of fines (FB) drifting in the water making the water yellow-ish. After those fines are also settled then you get the darker color because the bright fines are now all down. So it looks pretty normal what you describe.
Personally I keep repeating some A/B transits ( & filtering each acid state, finer filter each time) until the water above the settled FB is kinda clear (see pic below). Then I do my first manske. Just a habit of workflow.

The Grateful One said:
... I can't see your picture for some reason, Jees!...
You must have forgotten to pay your contributions? ;)
It does show on my screen, will attach here extra:

I generally let particles settle overnight (which is what I did with the beakers in the photo) which is why this process is taking several days. I just wanted to snap an early photo and share. :d The liquid above the FB became much clearer after sitting overnight, as usual. Nowhere near as clear as your photo but I am still getting the hang of this process, trying to find what works best for me. I appreciate all the feedback and advice!

However, it seems like I am losing product somewhere though because I am currently drying out the FB and it looks like it couldn't be more than 10 grams. Albeit quite pure, I'd imagine. Is it possible that sodium carbonate should not be used as the original base, but perhaps use it later in the process? I mean, it works, clearly but I wonder if it is as efficient as using lye first and then switching to sodium carbonate later in the process...just a thought. I believe lye is a more effective base, for sure, but I like to keep things food safe whenever possible. But I make exceptions sometimes...:d

Also, I saved the liquid from the original 5 boils and based it again. More harmalas precipitated! That seems to prove that I either:

1. Did not add enough base to begin with or

2. Sodium Carbonate will not effectively precipitate all the harmalas on the first go.

It should be noted that these are just ideas and by no means fact. When I get my pH meter it will make experimenting much more accurate and it will allow me to see where I might be losing alkaloids.

Edit: I also only do two Manskes.

:)
 
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