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Harmalas extraction-syrian rue (by SAKKADELIC)

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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

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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)

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


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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DoingKermit said:
Man that looks nice! Well done :thumb_up:
BlazingSatva said:
Looking good TGO!
Jees said:
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

Thanks guys!

I think 7 boils was probably over kill but there is no harm in that, obviously! ;)
Perhaps I'll write a song about this...call it "Squeeze the Seeds: The Downfall of Filtering"

:lol: :lol: :lol:

On a serious note, I will never go back to grinding rue seeds. This method is sound. I love it!

:love:

8)
 
The Grateful One said:
...Perhaps I'll write a song about this...call it "Squeeze the Seeds: The Downfall of Filtering"
...
I will never go back to grinding rue seeds. This method is sound. I love it!...
We actually still filter by squeezing, like a [filter + squeezing] in one action. "The downfall of gentle straining" is more puritan anal correct 😁

And yes grinded was yield-top before we got to squeezing, powder is now becoming more obsolete. I think that squeezing powder is a very messy job and for what possible gain? Perhaps I will try it once just for the academic sake of it, but with a gross course then instead of fine powder.
 
Jees said:
The Grateful One said:
...Perhaps I'll write a song about this...call it "Squeeze the Seeds: The Downfall of Filtering"
...
I will never go back to grinding rue seeds. This method is sound. I love it!...
We actually still filter by squeezing, like a [filter + squeezing] in one action. "The downfall of gentle straining" is more puritan anal correct 😁

And yes grinded was yield-top before we got to squeezing, powder is now becoming more obsolete. I think that squeezing powder is a very messy job and for what possible gain? Perhaps I will try it once just for the academic sake of it, but with a gross course then instead of fine powder.

:d

Indeed there is still some filtering going on (squeezing plus a couple times during the acidic stages). I'm just glad that I no longer have to watch rue tea drip painstakingly slow through a funnel with cotton balls and a coffee filter over and over (I don't own any cool filtration equipment, unfortunately...)!

"The downfall of gentle straining" ... :roll: :lol: :thumb_up:

I love this place, I really do!

:)
 
Results!

I gave a shot at finding out the utility of extracting harmalas from rue using a microwave and whole seeds. I have now run four extractions with this premise (the first two attempts being failures) and can say, that although it may not be the approach for everyone, I find that there are many advantages that make it worth considering.

In a nut shell, significant time savings over crushing seeds and/or boiling, similar to Jayrocco experienced with boiling whole seeds. I was able to obtain 4.7% and 5% fairly pure harmaline/harmine yields with a couple of hours labor, and a few overnights for soaking/settling/manske chilling.


Yields are about 20% less than mashing/boiling or extended boils with whole seeds. But, there is virtually no mess, no cotton balls or t-shirts. The first boils can be filtered through coffee filters. Only 90 minutes of cooking. Very clean results can be realized with a basify/rinse/manske/manske/basify/rinse and final rinse. I personally would prefer to extract 20% more seeds to avoid the process for crushed seeds.


Process:
- Soak seeds in vinegar acidified water for a few hours
- Freeze seeds
- Defrost in microwave
- Run 6 cooks in microwave at 15 min. each with vinegar acidified water and filter through wire strainer. (I lost about 200ml each cook to steam, so would add 400ml vinegar/water solution to filter off about 200ml from each cook)
- As each cook is filtered, run the solution through a coffee filter 2x
- Basify with a minimum of NaOH, decant and rinse
- Manske in minimum of vinegar and total of 400ml of solution

- Re-dissolve in hot water and Manske again
- Basify with a minimum of NaOH, decant and rinse, decant and rinse (to ph8 )
- Dry in pyrex dish an scrape up final yield

From 4oz (113g) seeds in each case:
 

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Thanks Sakkadelic--

It is all microwave cooking-- I edited my post to reflect this.

I don't have the beautiful yields of Grateful, but I like the 90 minute cooking time, and I only had to work with 1.2 liters of liquid. Since there is less cooking time I think I may get less 'gunk' in the brew.

Regarding the crystals, I followed Endlessness' advice to put the salt saturated solution in a heat bath (larger pot with near boiling water) to help it cool more slowly.
 
Was the microwave on high? what kind of container u were using during the boils? If i exceed 5 mins microwaving in a jar it will boil out
Regarding the crystals, I followed Endlessness' advice to put the salt saturated solution in a heat bath (larger pot with near boiling water) to help it cool more slowly.
I was gonna ask about that, i will try it next time for sure
 
5 % on whole seeds without squeezing them is really good :thumb_up:
Wonderful needles too.

Straining the seeds (as you did) or squeezing them empty in a T-shirt is IMHO same effort/trouble. I dare to believe that if you had squeezed them (all 6 times) then we had another member in the 6% FB club ;)
 
You may just be right, Jees. 😁 A twist in an old t-shirt would be worth the gain.

I will have to give those seeds a little hug next time and report any increased yields. It will have to wait a bit, though. After all the extracting, I have plenty of harmala for the near term.

I will keep monitoring this thread though-- I'm really enjoying all the good work from everyone.
 
Sakkadelic said:
Was the microwave on high? what kind of container u were using during the boils? If i exceed 5 mins microwaving in a jar it will boil out

My microwave is 1400 watts, and I did run it on high. Since the temps won't get above 100c, I figure the rapid boil is helpful, though I have no facts to back this up.

I used a Pyrex bowl with lid (about 1.5 liters) which is about 20cm across. I read in one of the MAE papers that a large surface area is preferable, perhaps it also cut down on boil-overs. I was able to combine seeds with 450ml water with lots of room to spare. The lid just sat on top to keep water from splashing out.
 
Very nice, Nitegazer! I like how quickly this can be done...I usually have to spread out my extractions over several days ( be it DMT, Cactus, Syrian Rue or whatever ) due to time constraints. For rue, I like to let it settle for at least 12 hours (for each stage that requires settling) so that is what was taking up most of the time! But hey, at least it isn't because of filtering anymore!

:lol:
 
I messed up on almost every stage of the extraction and i still got 5% hcl harmala yield.
after 1 mw boil, 1 freeze/thaw on 50 grams seeds, i did 4 10 mins mw boils with squeezing and mashing i lost around 1/3 of the first boil when pouring the liquid because i was using a glass casserole like Nitegazer did(which i think is the best boiling method so far) i had trouble pouring out of it the first time.
Then i basified with much less lye of what i usually use(the only step i didn't mess up) then i added 1 liter vinegar because i was too stupid thinking it's impossible for all this (looking like freebase) precip to be only plant material(which i think is what gives the original tea it's cloudiness) i should start counting on the colour change untill i get a ph meter.
Then i filtered and rebasified, did 1 water wash and continued to manske where i poured some of the reduced harmalas tea by mistake
Also i was working fast and only waited around 45 mins on each freebase settling stage the whole procedure was done in 16 hours first 4 were for first boil and freeze/thaw and last 6 were for slow cooling after manske plus sleeping, the filter was dried in less than 30 mins using a hair dryer.
so with only 4 boils, losing a significant amount of the liquid and working fast i still managed to get a satisfying amount of these beautiful gold xtals :)
The first picture is the second basifying stage after making the vinegar mistake, u can see how much vinegar i used the volume was around 200 ml before adding the 1 L vinegar and 300 ml water i even did 1 water wash before this to prevent using a lot of vinegar.
 

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Damn,

That looks great, Sakkadelic--

Only 40 mins of boil? I certainly must try pressing the seeds as you and Jees recommend.

One of the things I like about the shorter boils is that is seems that they make it easier/quicker to get a clean product.

From several days via the Tao of Rue to 16 hours via this method-- great work!
 
Thanks :)
I love the golden colour, there is a story about an arabic alchemist/scientist making a gold like material that gave it to the guard to escape from prison maybe it is hcl harmala if there is a way to make it solidify like gold.
Yeah u can see how the seeds get swollen it's all water, the water trapped in the end is supposedly from the last boil which doesn't have much alks but that's not the point i think the advantage of pressing the seeds is reducing time, the alks that needs long hard boils will go out by mechanical force...
I think 4 boils are not enough i got 2% less than good hcl yields and the quantities i lost when pouring and fast settling can't cover all the 2% loss so maybe a 5th boil is needed, i kept the seeds i will work on them later to see how much was left.
 
Just a quick question about the first post please. In the list of "resources" it doesn't have a quantity for the Rue, as I read the thread, there is quantities for the other resources, but not that 1. Any help much appreciated with this particular batch size.
 
Rigman said:
Just a quick question about the first post please. In the list of "resources" it doesn't have a quantity for the Rue, as I read the thread, there is quantities for the other resources, but not that 1. Any help much appreciated with this particular batch size.

It was mentioned in the "NOTE" above the resources, 50g or less of rue seeds :thumb_up:
 
Thanks a lot for the quick response Spaced Out, I didnt put 2 and 2 together with the quantity as I guess I was looking for more definition like a recipe (with a definite measure/amount for each item). Again, tha ks for the help ;-)
 
Rigman said:
Thanks a lot for the quick response Spaced Out, I didnt put 2 and 2 together with the quantity as I guess I was looking for more definition like a recipe (with a definite measure/amount for each item). Again, tha ks for the help ;-)

I didn't mention a specific quantity bcz in the later steps you add as much as needed of lye and vinegar and water...
I will rewrite this soom bcz i learned new things and some details need to be changed
 
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