• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Harmalas extraction-syrian rue (by SAKKADELIC)

Migrated topic.

Sakkadelic

Esteemed member
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

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

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.


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

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


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


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)

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


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.

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

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.
 

Attachments

  • 20150704_160501.jpg
    20150704_160501.jpg
    1.9 MB · Views: 9
  • 20180209_205903.jpg
    20180209_205903.jpg
    2.1 MB · Views: 8
  • 20180209_205540.jpg
    20180209_205540.jpg
    1.6 MB · Views: 8
  • 20180209_133849.jpg
    20180209_133849.jpg
    3 MB · Views: 7
  • 1455747813085.jpg
    1455747813085.jpg
    59.2 KB · Views: 7
  • 20160108_164526.jpg
    20160108_164526.jpg
    2 MB · Views: 7
  • 20160107_200952.jpg
    20160107_200952.jpg
    2 MB · Views: 7
  • 20150704_204646.jpg
    20150704_204646.jpg
    1.9 MB · Views: 7
  • 20150708_191425.jpg
    20150708_191425.jpg
    1.7 MB · Views: 7
  • 20150708_191320.jpg
    20150708_191320.jpg
    1.9 MB · Views: 7
  • IMG_8942.JPG
    IMG_8942.JPG
    1.3 MB · Views: 9
  • 20150727_192228.jpg
    20150727_192228.jpg
    2 MB · Views: 9
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)
 

Attachments

  • recovered+harmalas+jpeg.jpg
    recovered+harmalas+jpeg.jpg
    1.7 MB · Views: 0
Jees said:
: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:

69ron said:
Trickster said:
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?
 
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.
 
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
 
Jees said:
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! 😉
:)
 
The Grateful One said:
... 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 :?: )
 
Jees said:
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.
 
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:
 
Jees said:
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.

Jees said:
* 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:
 
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 😁
 
Jees said:
. 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:
 
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 ?
 
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:
 
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!
 

Attachments

  • harmala+harmala+harmala+jpeg.jpg
    harmala+harmala+harmala+jpeg.jpg
    3.3 MB · Views: 0
The Grateful One said:
...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)
 
Jees said:
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? :)
 
Back
Top Bottom