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Harmalas extraction-syrian rue (by SAKKADELIC)

Migrated topic.

Sakkadelic

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

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


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


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

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

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


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

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

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

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

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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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The best results i got were after doing acid-base-acid-base-water wash-acid-manske-base with minimal amount of lye-water wash
It looked very pure and almost white, too bad i don't have pictures i gave it to a friend to make changa
 
Okay, so I weighed my FB harmalas and it came out to 11 grams so far. I have more harmalas from this extraction after basing the original boils for a second time. If I were to estimate, I'm guessing the total yield will be anywhere from 15-20g freebase harmalas from 300g whole syrian rue seeds...I will post the actual final yield in a couple days when I am completely done with this extraction and have exhausted the starting material! Here is a pic:

Edit: Not the greatest yield (but I'm not complaining) and also the flash from my camera made the harmalas look whiter than they actually are. It is more of a light tan than white.
 

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They look good, good work :) i once was out of vinegar at midnight and needed a little more so i used apple vinegar and the solution turned dark and the freebase was brown i was working on a small quantity trying to determine how much was left after the main extraction and i threw it away.
so the only problem u had was not basifying enough?
 
Sakkadelic said:
They look good, good work :) i once was out of vinegar at midnight and needed a little more so i used apple vinegar and the solution turned dark and the freebase was brown i was working on a small quantity trying to determine how much was left after the main extraction and i threw it away.
so the only problem u had was not basifying enough?

Thanks! 8)

Yes, I believe my main issue was not keeping track of the pH throughout which led to the accidental discarding of alkaloids, likely during the basing steps. I am glad that I kept the liquid from the original boils, because there was/is alkaloids left over.
 
I'm trying this method on another non active plant and while working i got this idea to make it somehow cleaner and use less toxic materials(lye).
So let's say we did the acidic boils and some simple filtering (metallic mesh and cotton bag like jees proposed) then we basify and wait for settling. now we poor the high ph water but we don't discard it since we can use it to basify again using very little more lye if needed (when doing the normal extraction i noticed that i use less lye in the later steps of basifying) and of course we can filter this basic solution before using it to make it more clean.
if the basic water of the first base phase is not clean enough we use the second one....
I haven't tested it yet but it seems good to me maybe there is something wrong i'm missing...
So what do you think guys?
 
Look dude i u haven't noticed i wrote this tek i got high and clean yields from the first time i tried it and that's why i wrote it and i'm pretty much aware of what i'm doing. what we are trying here is to make it better
 
Sakkadelic said:
Look dude i u haven't noticed i wrote this tek i got high and clean yields from the first time i tried it and that's why i wrote it and i'm pretty much aware of what i'm doing. what we are trying here is to make it better

Lye isn't problematical whatsoever in the residual amounts of a proper tek. You arent improving anything, just making it longer winded.
 
Why did u delete ur comment and only left "Mmmm" i really don't know much about lye and sodium toxicity or how much is left in the product but as u can see a lot of people don't like to use it and the other replacement such as sodium carbonate which needs some work before use (heating in stove on a specific temp) and it doesn't work that well as we saw in what TGO did so it might be an improvement to someone who is worried about using much lye
 
Sakkadelic said:
Why did u delete ur comment and only left "Mmmm" i really don't know much about lye and sodium toxicity or how much is left in the product but as u can see a lot of people don't like to use it and the other replacement such as sodium carbonate which needs some work before use (heating in stove on a specific temp) and it doesn't work that well as we saw in what TGO did so it might be an improvement to someone who is worried about using much lye


Good points. Sorry i edited previous post cos i was stating the obvious, that the biggest issues were 1, getting the alkaloids out of the seeds as efficiently as possible, and 2, proper base use, and proper use of various purification teks/mankse, on offer in the wiki.

You offer a 'tek', as in use a microwave to extract whole seeds, but that's all- the rest is a copy of any of the other teks on offer from other people. Not everyone has a microwave, and lye is easier to obtain and probably better to use, than sodium carbonate.

A decent few boils of seeds in sufficient water with proper wringing out or mashing should get all the alks out of the seeds, microwave or not. And decent washing of product should yield a pure enough result where Naoh isn't a justifiable cause of any concern, especially in the typical tiny doses required in experiments.

In fact you could say use a microwave, or boil, and mash seeds, 3 times, etc to get a clean extract, then follow whichever tek on the wiki.:twisted:

Just my 2 cents 😉
 
For people who think this method is not an improvement
"use a microwave, or boil, and mash seeds, 3 times, etc to get a clean extract, then follow whichever tek on the wiki."
Thank u ganesh for ponting this out :)
 
Sakkadelic said:
For people who think this method is not an improvement
"use a microwave, or boil, and mash seeds, 3 times, etc to get a clean extract, then follow whichever tek on the wiki."
Thank u ganesh for ponting this out :)

Well, it IS an improvement on the INITIAL liquid extraction phase, the rest follows known protocol. I'm offering praise where due, but in sincerity, there is no limit to improvements especially purity. All at the cost of time, materials, and of course yield.

Your first post was excellent. I just don't know why you then bother using Sodium Carbonate instead. I know some pple like using it, but personally i believe they are misguided doing so.:thumb_up:
 
I never used sodium carbonate or said that it should be used. to me the only ideas i added was going for whole seeds which reduced a lot of work to get a pure product, mashing and applying force to drain seeds there is also a good reduction of time...
the only thing i changed in the original post was the freeze/thaw after each boil
 
ganesh said:
...A decent few boils of seeds in sufficient water with proper wringing out or mashing should get all the alks out of the seeds, microwave or not...

Well, the jury is still out there how much the micro's can contribute:
link

It could be an academic truth without much practically impact, yet it might do more.
Even if micro's lead to same amount of product but in a shorter (economic) time and/or power input then this is already worth something.
 
My grand parents were in Iran doing religious things and i asked them to buy some for me, it's really that cheap there and the quality is good. the first batch my mother got it for me from there too :)
 
Sakkadelic said:
My grand parents were in Iran doing religious things and i asked them to buy some for me, it's really that cheap there and the quality is good. the first batch my mother got it for me from there too :)

Well done for asking for some. It's amazing how cheap these plants are at source. I bet the main vendors get them at similar rates too.
 
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