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Harmalas extraction-syrian rue (by SAKKADELIC)
- Thread starter Sakkadelic
- Start date
Why don't you try what was described already? If you report your results and experience here, Sakkadelic might use the feedback for his improved version.
Rigman said:
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
It sort of ruins the nicely looking crystal shards, but it does take out a lot of residual salt-laden moisture.Sakkadelic said:
Rigman said:
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
greyexplorer
Rising Star
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.
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 helpfulgreyexplorer said:
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).
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).
doubledog said:
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.
doubledog said:
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.
Attachments
BongQuixote
Rising Star
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.
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.Loveall said:
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
Attachments
merkin
Rising Star
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)
. 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)
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
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
merkin
Rising Star
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.
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.
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.
Attachments
merkin
Rising Star
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.
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.