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Harmalas extraction-syrian rue (by SAKKADELIC) Options
 
Sakkadelic
#1 Posted : 7/31/2015 10:27:02 AM

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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.
Sakkadelic attached the following image(s):
20150704_160501.jpg (1,958kb) downloaded 2,349 time(s).
20150727_192228.jpg (2,049kb) downloaded 2,346 time(s).
IMG_8942.JPG (1,334kb) downloaded 2,337 time(s).
20150708_191320.jpg (2,006kb) downloaded 2,339 time(s).
20150708_191425.jpg (1,794kb) downloaded 2,327 time(s).
20150704_204646.jpg (1,976kb) downloaded 2,323 time(s).
20160107_200952.jpg (2,089kb) downloaded 1,254 time(s).
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20180209_133849.jpg (3,109kb) downloaded 840 time(s).
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20180209_205903.jpg (4,834kb) downloaded 839 time(s).
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 

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Sakkadelic
#2 Posted : 7/31/2015 10:53:12 AM

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sorry for the rotated images, i tried to make every picture fit between the steps but it didn't work
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
AcaciaConfusedYah
#3 Posted : 8/1/2015 12:19:23 AM

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Excellent! The Microwave movement grows! I will give it a shot on my next harmala extraction. Well done, and i think you have earned a Vote for Promotion.
Sometimes it's good for a change. Other times it isn't.
 
Sakkadelic
#4 Posted : 8/1/2015 1:24:56 PM

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thank you ACY Smile
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
smokerx
#5 Posted : 8/4/2015 4:18:17 PM

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Thank you very much for all that good work.
We are each of us angels with only one wing, and we can only fly by embracing one another.

*********

We are all living in our own feces.
 
null24
#6 Posted : 8/4/2015 4:56:26 PM

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ThanksThumbs up

I'm about to embark on my first syrian rue extraction, and may use this method!

Couple questions, is the freeze/thaw just for cell lysing, and if so, couldn't it be replaced with grinding the seeds?

Also, not trying to be picky, and maybe i read wrong, am misinformed etc, but wouldn't it be an acetate, not HCl in step 5b?

Good work man, you were promoted before i got a chance to vote you up, so here's a Thumbs up
Sine experientia nihil sufficienter sciri potest -Roger Bacon
*γνῶθι σεαυτόν*
 
Sakkadelic
#7 Posted : 8/4/2015 7:07:47 PM

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thank you guys Smile
i tried to avoid grinding the seeds because it will leave you with a lot of impurities in the solution and it's not like DMT extractions where the plant material don't get mixed in the solvent, maybe step 3 can still solve this problem, i never tried it with grinded seeds but i will soon for you if you believe grinding is better, it could be.... and if you don't have a very fine metallic strainer a lot of the plant material that didn't get boiled enough will escape to the jar

yes the freeze/thaw is just for cell lysing but i do for another reason, at first i tried to do 5 consecutive boils but i realised that the short boiling time in the microwave is not enough, so it's good to wait few hours between boils and i thought that to mash, freeze, thaw and boil will extract more than just leaving the mix on the table for the same amount of time then boil.
this whole thing is just to avoid using the gas stove for many hours.

you could be right i'm not sure if it's acetate or hcl but i highly doubt that the guys here can make such mistakes, everything i learned about rue extraction is from this site.
https://wiki.dmt-nexus.m...he_Tao_of_Rue_Extraction
in this tek, step 5, they said "After you have decanted the basic (high ph) lye water off the top, you want to add some hot vinegar and water to your freebase alks to redissolve everything back into the solution as harmala acetates."
and in step 6(manske) they mentioned"It's better to use one of the above methods, preferably Phlux's on the final manske and push any remaining alks out by reducing the solution further after you filter the harmala hcl."
and in step 7 they also called the filtered crystals harmala hcl.

i hope this was helpful to you i only did this method few times and it worked great even from the first time that was also my first rue extraction, a lot of modifications can be done to reduce time and get higher purity, i still need to try few things and maybe you can help with that Smile
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
brilliantlydim
#8 Posted : 8/7/2015 10:19:02 PM

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Is microwaving a must? I got rid of mine a few years ago with no plan on getting another.
 
Sakkadelic
#9 Posted : 8/8/2015 12:44:17 AM

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ehud wrote:
Is microwaving a must? I got rid of mine a few years ago with no plan on getting another.

the first step acidic boiling can be replaced with any acidic boiling in other teks
it usually goes like this:
add water and vinegar to the seeds.
you freeze/thaw a couple of times(no need to repeat this when you repeat boils).
boil for an hour on a stove strain the seeds mash them and repeat 5 times.
you just need to figure out the amount of water you have to add because a lot of it will evaporate this way but don't worry i don't think it'll make a big difference
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
Nitegazer
#10 Posted : 8/20/2015 2:18:20 PM

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Just another 'thank you' for this tek. I'm a big believer in microwaving into solvents, and this is a great application of that approach.

I will be running my first rue extraction in a couple weeks as the first step to THH synthisis, and I am hoping for as high a harmala yield as possible.
 
Sakkadelic
#11 Posted : 8/20/2015 3:45:29 PM

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thank you Nitegazer and big thanks to AcaciaConfusedYah, i started using the microwave after i read his microwave assisted drytek
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
JustCurious.
#12 Posted : 8/31/2015 6:50:09 PM

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Nice Smile

 
Sakkadelic
#13 Posted : 8/31/2015 8:43:29 PM

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thank you for clarifying this JustCurious. and null24 Smile i'm too stupid for not noticing this but there's something wrong in "the tao of rue extraction" they said they used vinegar but they wrote hcl and the shape and color of the crystals in the images are different than what i got
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
BongWizard
#14 Posted : 9/2/2015 1:08:42 PM

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After the manske, your harmalas will be in the form of hydrochloride salts. While you are correct that adding vinegar to freebase harmaloids will cause them to dissolve as an acetate, the use of NaCl to saturate the aqueous solution causes chloride ions to supplant the acetate radical (owing to their difference in electronegativity), thus forming the HCl salt, which precipitates when cooled.

So you were right the first time. Remember, "the path of the Tao is not always the easy one, but it is always the right one."

I hope that clears things up.

EDIT: oh, one more thing. If you grind the seeds, this method won't yield clean product. Fine particulate plant matter will remain in the solvent after decanting. It's for this reason that extractions from rue tend to focus on filtration.
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


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Sakkadelic
#15 Posted : 9/2/2015 3:47:35 PM

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thank you BongWizard i was right but i didn't understand what's going on until now Smile
do u have any idea why the crystals i got have different shape and color?
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
BongWizard
#16 Posted : 9/3/2015 2:10:15 AM

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The difference in your crystals is due to contamination by fat, tannins and, possibly, a small amount of vegetable matter. What I would recommend adding is one step of filtration.

After redissolving your freebase harmaloids in vinegar, filter the resultant solution before adding NaCl to manske. It's at this stage that any fats/tannins are removed.
"Laws alone can not secure freedom of expression; in order that every man present his views without penalty there must be a spirit of tolerance in the entire population." -Albert Einstein


I'm not a big fan of SWIM. I mean, I've never met the guy, but any time I hear about him, he's doing something sketchy.
 
Sakkadelic
#17 Posted : 9/3/2015 6:15:38 AM

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I will definitely try that next time Smile
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
Jees
#18 Posted : 9/3/2015 8:21:26 AM

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Sakkadelic wrote:
... i never tried it with grinded seeds but i will soon for you if you believe grinding is better,...

If you get 6% yield with not grinding your seeds, stick with it, this is very neat.
Filtering grinded seeds is a pain in the aarsche, I made a thread how to overcome the problem but then it take a ton of time and still same 6% yield. I gonna try your freeze/thaw micro style a go on whole seeds to compare. Thx for posting. Thumbs up
 
Jees
#19 Posted : 9/14/2015 5:07:38 AM

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As promised, I gave some of the ideas here a try on whole seeds with good result, except for:
• My old microwave makes too many hot and cold spots, so went for simple old fashion boils;
• No fitting potato masher so I used another kind of force.

From whole seeds the yield was amazingly 7.1% rueHCL (or 6% freebase).
Same batch seeds with the "grind workflow" gave 1% less.

The two main factors that differed from the grind-workflow were:
• 5 x freeze/thaw with a good dash of vinegar, never did freeze/thaws before;
• Exerting much of force on the seeds to squeeze them empty several times in the process.

In short it was:
• 5 x freeze/thaw in 50% water 50%vinegar, moisture till some free liquid is visible, the liquid was never replaced. 5 Is what I did, perhaps less is as good enough;
• 5 times a 30 min boil with only 1 cm level above seeds level, each time a dash vinegar present;
• After each of those boils a cool down till touch warm, poor seeds in a very thin cotton kitchen towel, make a ball with the seeds and twist the towel above the bowl so the bowl gets compressed as you twist. Twist as hard as you can, then start squeezing the ball with your hands as hard as possible to empty the seeds. Collect liquid in a pot. Poor the squeezed seeds in the boil pot, they are fairly semi-dry now. Add new water (+ soup spoon vinegar) till 1 cm above seeds level, boil for 30 minutes, repeat… so you end with 5 times collected liquid.
• Base the pot with collected liquid and proceed as usual.

I think the squeezing part with the towel beats any potato masher, it would have simply bend compared to the forces exerted with the towel. With the towel you simply apply all the muscle power of your arms/hands available to empty the seeds as max possible.

The liquid from this workflow is clearer than workflow grind-seeds, that is a plus for the rest of the process.

Yield wise I see no further benefit in grinding from here, only if grinded was obtained I would use it.

So thumps up for attacking the whole seeds with the freezer and brute muscle power.
Thumbs up
 
Sakkadelic
#20 Posted : 9/14/2015 10:46:32 AM

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I'm so glad u tried it Smile thank u.
Yes the towel thing seems amazing i can imagine how much more power can be applied. I have a strong and big metallic strainer so i go hard on them too.
if u noticed i don't freeze 5 times anymore it's not necessary i just mash, boil and strain/squeeze....
i like the way u work and ur creative ideas in all your posts Smile
I really think this method can be reduced and simplified much more i will try to modify and reduce the time of the steps...
"Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
 
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