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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.

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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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merkin said:
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 no matter how many times I 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.

As a follow-up, I based the gunk what dissolved below pH5.5 with sodium carb and it crashed as a brown precipitate, so it would survive the usual A/B steps.
 
Hi people
This is my first go at this Tek by SAKKADELIC
I just finished step 5,looks good. BUT has a bad taste to it.
I took some photo's an d when I zoom in you can see white stuff (caustic soda) ?
in step 4 I water washed 5 times the PH was 12.I don't know how many times two wash it
I need to know my next steps In detail
So do dissolve it in vinegar and do more water washers and how low should I go with the PH.
 

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Hi michaeljohn1234m,

these are harmala hcl crystals obtained by manske so there is no way they are contaminated with caustic soda. one very likely contamination is salt.

they are supposed to taste bitter and bad in this form. the freebase is tasteless when pure in my experience.

your results look great from the pictures :thumb_up: . what was the yield?

if you'd like to further purify it:

-dissolve in warm water and a little bit of distilled white vinegar.
-basify with sodium carbonate, after basification with only sodium carbonate the solution remains yellow, this is fine but you can add a few drops of caustic soda solution and this will complete the conversion
-top the container with water, let settle, decant. do a couple of washings. you can collect the harmalas as freebase at this point.
-if you'd like to have the hcl crystals. you can repeat the manske step.
 
Hi Sakkadelic
That's good news. I thought they were suppose to be tasteless, but that's step 6.
I got 7g from 100g of seed and it looks great.
your tek is so much easier. I did 15min microwaves. 5 times, got it all out.
I'm going to use it with DMT. So what I'd like to know is,Do I use it as is or should I go the next step and free base it, or both steps back to hcl crystals.
and thank you for all the Time you have put into this Tek and the others who contributed
 
Thanks! glad it worked out well for you.

7% harmalas HCl is a very good yield! and it looks clean. it is probably contaminated a bit with salt but that is fine.

if you use it orally in capsules, it doesn't make much difference whether it's harmala salts or freebase. The freebase however is heavier so 100 mg of HCl harmalas =(in effect)= 85 mg freebase harmalas. you need to adjust your dose accordingly.

the freebase is more versatile, it can be used sublingually with minimal taste, it can be smoked on its own, infused in leaf, or used to make changa. but if it is not stored properly it degrades and turns red, the HCl harmalas is more stable and stores better.
 
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