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Harmalas extraction-syrian rue (by SAKKADELIC)

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Sakkadelic

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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

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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.

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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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Rigman said:
Sorry to keep posting in your thread Sakkadelic, do you have an estimate of when you may be updating this as I am really looking forward to giving this a run.

Hopefully this weekend i will
I'm not gonna change much, gonna make it more general, no more jars and sizes.. add some notes and i used to use too much lye so i will change that..

@pitubo
You mentioned in a post to use tissues to dry the harmalas after manske to minimize salt contamination, i used tissues for drying but i never thought it served that purpose too so thanks a lot for pointing that out
 
Sakkadelic said:
You mentioned in a post to use tissues to dry the harmalas after manske to minimize salt contamination, i used tissues for drying but i never thought it served that purpose too so thanks a lot for pointing that out
It sort of ruins the nicely looking crystal shards, but it does take out a lot of residual salt-laden moisture.
 
No problem Pitubo, I was planning to do it as described until Sakkadelic said that it was going to be updated, so I figured if it was being updated soon I would wait for the new version, if not I would move forward as is.
 
Rigman said:
No problem Pitubo, I was planning to do it as described until Sakkadelic said that it was going to be updated, so I figured if it was being updated soon I would wait for the new version, if not I would move forward as is.

I updated the tek, hopefully it's better now, i just felt it was poorly written maybe it's not much better now but i feel better about it.

If u still want to know how much to start with i suggest to start with 35grams and aim for a 2g yield.

Please if you could give a feedback whether it's better now or not and if there is anything unclear please tell me :)
 
Many thanks to Sakkadelic for the thread!!

Step 4, Basifying and water washes. "Refill the jar with water".

Since there were no previous steps where just water was used, I need to ask, are you saying plain water, acid water or base water?

Thank you.
 
greyexplorer said:
Many thanks to Sakkadelic for the thread!!

Step 4, Basifying and water washes. "Refill the jar with water".

Since there were no previous steps where just water was used, I need to ask, are you saying plain water, acid water or base water?

Thank you.
heyyy! i am glad it was helpful

yes plain water, after you decant the basic water, inevitably some of the basic water will be left behind.. so you need to keep diluting it with plain water until it is safe to use..
in step 4, the reason for the wash is to dilute the base so we don't have to use a lot of vinegar to reacidify the solution.. in step 6 the water washes are much more necessary to obtain a safe to use product.

btw i edited the post a bit.. nothing major just little things

also i will be adding a new better method to remove more of the water at the last step before drying the freebase
 
This remains my favorite TEK to end up with clean harmalas.

I have one question,

- Is the first basing important to be done with NaOH instead of Na2CO3?

When acidifying after the first basing, some impurities are no longer soluble. I think these are denatured plant material. If so, using NaOH may do a better job at "denaturing" than a gentler base.

As far as yields go, I believe Na2CO3 is strong enough to crash the harmalas as shown in the VDS protocol. Na2CO3 could be used in the steps after using NaOH once (where the purpose of using NaOH is denaturing/cleanup).
 
My experience is that hydroxide is better because separation/precipitation is quicker and cleaner. Using carbonate is quite messy with rue tea, at least ime. I used carbonate just once and will never repeat it.
 
doubledog said:
My experience is that hydroxide is better because separation/precipitation is quicker and cleaner. Using carbonate is quite messy with rue tea, at least ime. I used carbonate just once and will never repeat it.

I just did an experiment that goes along these lines.

I had some sodium carbonate crashing, harmala seemed done precipitating (got a bunch quickly, then the solid layer stopped growing). However, the water was still cloudy. Poured off some of the cloudy water and added NaOH. The cloudiness crashed a lot faster than the remaining liquid in the original sodium carbonate jar.

Then I acidified the NaOH jar with the new precipitate. Nothing much seemed to go into solution at all. I think whatever was making the sodium carb solution cloudy was a contaminant that NaOH crashed quickly and "denatured" so that it would remain solid and separate out furing the acid step.
 
Interesting, this means that sodium carbonate precipitate is cleaner because this contaminant has not precipitated.
I always thought that crashing with hydroxide is more complete, but it seems that main advantage is just speed.
 
doubledog said:
Interesting, this means that sodium carbonate precipitate is cleaner because this contaminant has not precipitated.
I always thought that crashing with hydroxide is more complete, but it seems that main advantage is just speed.

I did another experiment: after several A/B (vinegar/NaOH) and two makes, I had yellow clean looking HCl salts. I dissolved them in water and based carefully with ammonia drops and a pH meter, stopping after the second pH drop/rise depression, when harmaline finishes crashing per the VDS protocol.

After separating out the harmalas with a filter as usual, I added NaOH to the filtered liquid. White stuff crashed. It dried to flakes (see image). Harmalas dry to a crust that becomes a powder when crushed, this seems different and more flaky. It is a small amount (650mg), about 10% of the bulk harmala weight, but is did survive all the other cleanups.

So stoping the pH rise once harmaline precipitation is complete may be useful as a cleaning step (compared to bombing with NaOH). Harmaline precipitation can finish at a pH as low as 8.5 per the VDS protocol.

I wonder if when acidifying to dissolve the FB as a salt there is a similar situation. Perhaps lowering the pH below 3 helps dissolve unwanted stuff. Maybe tracking the pH as vinegar is added to water and the harmalas go into solution could be used as an indicator. Perhaps at pH 5 harmaline and harmine are both in solution and more contaminants can be separated by stopping at a milder pH.

In short, there could be a smaller pH range that still yields well and at the same time helps keep contaminants out.
 

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You may want to try a few more manskes. I find that most garbage crashes out in the third manske, and I usually do five to be sure. It could also be the "mixed" portion VDS talks about, so that would be a harmine/harmaline mix, but I don't see why it would look like that.
 
Loveall said:
This remains my favorite TEK to end up with clean harmalas.

I have one question,

- Is the first basing important to be done with NaOH instead of Na2CO3?

When acidifying after the first basing, some impurities are no longer soluble. I think these are denatured plant material. If so, using NaOH may do a better job at "denaturing" than a gentler base.

As far as yields go, I believe Na2CO3 is strong enough to crash the harmalas as shown in the VDS protocol. Na2CO3 could be used in the steps after using NaOH once (where the purpose of using NaOH is denaturing/cleanup).
Haha thanks Loveall, I plan to update the tek someday but I still encountered weird stuff on my last extraction and I am not having time to do more kitchen experiments.

Yes, i always noticed this gunk that results from basing with NaOH and refuses to redisolve with vinegar. And I suspect it to be the thing that makes filtering harmalas a pain. So basing with NaOh is a good cleaning step.

I like to use Na2CO3 for the final basing if I want to keep the freebase and I also add a few drops of strong NaOH solutiom to eliminate the yellow color from solution that remains after basing with Na2CO3, and a couple water washes after that. There's not much harmalas left in there but this results in purer looking harmalas.

Recently I wanted to try eliminating the gunk even before the first basing by just washing the seeds. I started with 75g seeds and I did several cold water soaks and 2 hot ones and I collected the water. I added NaOH and a lot of gunk precipitated, I cleaned the stuff as much as I could and only a tiny amount of harmalas was in there (70 mg) the gunk was 700 mg. I added pictures of the gunk.

More gunk came later in the extraction so washing alone is not enough to remove it, but I think it is useful to do a soak and discarding the water at the beginning. I don't know if that could help when drinking rue but I'll be doing a soak and some washes before preparing the tea whether for drinking or extraction.

Very interesting what you observed in the last post. The flakiness reminded me of the mysterious blobs i got in the past. These blobs survived 2 A/B cycles and a manske. If you identify the substance you got please let me know.

Thank you Loveall for all the beautiful work you do
 

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Having just received a kilo of seeds from the east I undertook to try Sakkadelic's tek, especially since it has Loveall's approval :) . Seemed better and less laborious than what I'd been doing before and processing 200g in two batches took a long weekend (with settling) instead of weeks previously! Wanted to go up to before Manske but not further since I would like to try the "full spectrum" (much as I love seeing manske crystals).

Anyway, suffice to say I am impressed! Had a mate arrive in between batches and he did the squeezing on the second batch. He has much more impressive arms than me and it shows in the results. 'The Squeeze' should not be underestimated! Also he destroyed two patches of cloth filter...yield in total was slightly under 10% which I think is pretty good (for me anyway)

My questions -
-What is oral dosage of this? (for a 'by-itself' rue experience and also for vaping spice).
-Is one pass base - acid - base enough for oral cleanliness of full spectrum? Or should I do another round?
-Approximately what % is harmine and harmaline out of this? ie roughly how much can be expected to disappear after the first manske?

@Sakkadelic - thanks for this - my least painful rue extraction ever!

Some pics. I love threads with pics, so for everyone else who does....

(Note: After overnight drying alks in a dehydrator the final yield was closer to 8% - 17,688)
 

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hey merkin,

thanks for trying the tek, I'm happy you got good results with less effort. I am trying to think of a way to make the squeezing easier and less messy, hopefully i come up with something soon.

one pass base - acid - base is good enough as long as you did the water washes at the end. 10% is higher than what is typically reported with rue seeds so regarding dosing I would would take the equivalent of 3-4g seeds for a full experience but start with a lower dose in case your seeds were unusually high yielding.

the percentage of harmine and harmaline would depend on the alkaloid profile of your seeds. I tried the crude separation method the other day and got around 50/50.

In principle you should only lose 5% of the alkaloids with manske, which you can still recover. both harmine and harmaline will crash with manske. but your 10% yield will probably drop to about 5-6%. use only 15g/100ml salt and not as I mention in the tek. this will minimize the salt contamination.

good luck :love:
 
Yr welcome, I enjoyed this tek a lot.

Makes sense to estimate dosage based on a 'raw' rue tea. Didn't think of that!

I have done this process a few times in the past, exploring the VDS revelations and methods all the way to doing a THH zinc reduction.

The big difference here for me (apart from microwave and freezing) was basing the pulls without first reducing and settle/decanting the pulls plus running some filter steps on the pulls (which took forever). This tek led to the fastest and cleanest "first full alkaloids" batch I have ever seen before doing the manske. Usually they were much much darker in color too, so that was nice.

Since reading around nexus about using 'full spectrum' rue I am keen to try that as opposed to the purer harmine/harmaline separations to see if there is a perceptible difference in both oral/sublingual and vape/changa. I wasn't too sure if the tan color was still too dark for safe oral and maybe needed to get whiter. I did water wash till pH dropped around 9.4 (my water 8.76) so I figured it was quite close to good. Passed your 'slippery finger' test.

I dried the alks in dehydrator low overnight and a bit of weight disappeared - leaving the yield closer to just over 8% (17,688g from 200g). There's still a bit to process after a final boil of the combined "spent" seeds for an hour in a pot, but I don't expect too much - its settling now and liquids were significantly yellower than the dark red/tan ones above - indicating saturation I guess - but it will probably push the yield over 18g.
 
Thanks Sakkadelic. Good to hear your results merkin.

I went ahead and tried acidifying harmala FB with a pH meter;

- Freshly filtered harmala FB (~6g) was moved into a new jar (filter and all, didn't bother drying beyond squeezing).
- 400ml of water added
- pH measured 9.5
- Started adding vinegar. Withing a few seconds pH would drop, and then increase as harmalas went into solution. I didn't wait to reach equilibrium, I just added vinegar and verified pH dropped and continued to increase.
- This kept on happening, until I noticed the pH stopped increasing. The pH meter was at 5.5 at this point. I may have been able to end up a little higher. A possible approach is to go to pH~ 6, verify pH increases, and keep on adding vinegar until the pH stops bouncing back, trying to end with as high of a pH as possible.
- I filtered the solution. A lot of gunk was not dissolved and caught by the filter. The color of the solution was yellow/orange, not the typical red (left jar in image below).
- To test if some of the gunk in the filter could be a "new catch", I tried to dissolve it in vinegar (pH~2.7). A lot of it of it did. The solution it made looks brown (right jar on image below).

What could be going on is that in the pH region between 2.7 and 5.5 gunk that we don't want becomes soluble. Targeting the pH during the acid step as high as possible (~6) while not seeing the harmala "bounce back" (indicating harmalas are done dissolving) could be beneficial to separate more impurities.
 

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That's an interesting observation Loveall. I have always found that no matter how often I filter the acid liquid going from a-b (also including manske steps) there always seems to be more dark stuff in the filter. I don't filter the base liquids unless collecting precipitate, usually just a decant/siphon.

The pH is obviously varying a lot when I'm doing these but I have tended to go quite a lot lower (<4) and often even lower. I was not paying attention to it at all when acidifying really - most of the time I was watching pH in detail was during the basing for separations and pH reversals, never the acidifying.

This is probably the reason the acid phase cleaning filters always seem to leave yet more stuff no matter how many iterations! I suspect you are right that controlling it and keeping it in a tighter range is a good idea.

**OT
As an aside, I bioassayed 300mg of my 'full spectrum' and it kicked my butt! Bit strong for me but quite stomach trouble-free apart from a sudden urge-to-purge around t+2hr but the purge was done and dusted v quickly with no nausea build-up or die-down like my full rue 'tea' experiences.
 
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