Manske Tek Intermediate and Final Step Questions

[aethereon]

This is a quasi continuation of my older post regarding harmalas extraction using the Tao of Rue manske tek. Some people reccomended going with Sakkadelics harmala tek but i guess i am stubborn or crazy or something and kept doing the manske tek. The dunning-kruger effect is definitely real, I thought after doing it about 4-5 times I was becoming "a pro" (so i thought) getting 'crazy yields' with my vac rig... The vac filtration defnintely helped a lot. I did an extraction where i filtered like crazy for what felt like days, at the end of it netting some pretty nice(or so I thought) harmalas.

But then I realized, I'm still such a noob at this. My big question is what is the big difference between base precipitated harmals, vs salt precipitated harmalas, if any?

Why does the tek(s) reccomend at the last step going with another base precipitation?

I kinda just stopped at the salt precipitated needles omiting the whole lye/sodium carbonate last step and was thinking I'm all good(or good enough) but my latest batch didn't seem to have that much 'oomph' to it. Perhaps this could be a different topic on the subject, I've heard there is a reverse tolerance with Harmalas but I've just think I've gotten regular tolerance. Is there like a difference in bioavailabilty or chemistry with the two different precipitations? Is it okay to just stick with the salt precipitated harmalas or is there a reason to go with the base as the last step? Also one other question, how does one wash harmalas? Perhaps this is the key, somewhere i remember reading that salt-precipitated harmalas are quite water-soluble and i'm thinking washing means rinsing with water? Preferrably cold? Cause yeah i did feel like washing the 'salty' ones was potentially reducing my yield (via dissolving some of the yield during the wash.) Also one other question, what happens to the remaining NaOH when one redissolves the basified/decanted harmalas with vinegar... i'm guessing alkalinity wise it becomes neutralized, but are there any sort of 'chemical' leftovers from using NaOH one should be worried about?

Anyways any feedback/ideas would be greatly appreciated, thanks

 

[Sakkadelic]

Hi aethereon,

The main difference is regarding what you plan to do with it, here's some cases.
-for smoalking you should use the freebase.
-for oral ingestion it doesn't matter much, the stomach acid will convert it to a salt form anyway.
-for sublingual both would work but the salt form is very bitter while the freebase is nearly tastless.
-for long term storage the salt form is more stable, freebase harmalas can turn into the mysterious haramala red.
-for accurate dosing the freebase is better as the manske produced salt might be contaminated with salt (NaCl).

Regarding the washing, it's meant for the freebase and it as simple as topping the container with water, waiting for the freebase to settle and decaning the water. Harmala salts are soluble so they cannot be washed with water.

When acidifying a lye solution, the NaOH is turned into a sodium salt + water, and it will stay in solution when you produce and collect the harmala salt, there might be trace amounts trapped in the water that the filter absorbs but nothing to worry about. In any case, dilute NaOH is not harmful and is used in food products.

You should worry about NaOH when you want to produce the freebase. To deal with it, first thing is to not use excessive amounts of NaOH, and then doing water washes to make sure the NaOH is diluted to the point where no harmful amounts are left when drying the freebase, and remove as much as possible of the water before drying the freebase. You can also do the final basification with sodium carbonate mainly and only use a few drops of NaOH to drive the PH higher so the solution is no longer yellow, followed by water washes.


The trick to an easier harmala extraction is to directly basify the rue tea before any filtration, and then do multiple water/base washes and decanting, this will get rid of most of the sludge that makes harmalas hard to filter. You can then do a crude manske step. After that you can continue the way you want and filter the solution during an acid step to get rid of any undisolved material.
making the rue tea with whole seeds is also less messy and reduces the sludge and other contaminants.

 

[aethereon]

This is incredibly amazing, huge smile on my face... thank you, very informative. I definitely noticed the taste is definitely "bitter" I was really wondering how people do that. Perhaps I just had a bunch of salt in mine as well in regards to the 'potency.' I appreciate all your points Sakkadelic. The only one point I am not clear on is when you said "drive the PH higher so the solution is no longer yellow, followed by water washes" Do you mean when adding the base to the solution, it turns yellow, and you should add a bit more? I remember it going a bit more 'milky white' beyond that point, if memory serves me correctly is that what you are referring to?

Thanks again, and amazing quote in your sig.

 

[Sakkadelic]

You're most welcome aethereon, I am glad it was helpful and it puts a big smile on my face too!

yes you're right, the color change is not as clear in the initial stages of the extraction. in the first basification step after the harmalas had settled the solution on top remains brown, at later stages the color will be yellow, and finally when the haramalas are clean the water above them should be colorless.

the idea of using sodium carbonate and few drops of NaOH solution is meant for the very final basification step if you're desired end product is the freebase. at that stage the harmalas should be quite clean and the color change is easier to observe. so if your harmalas are dissolved in an acidic solution the color should be a good yellow/orange. If you basify with sodium carbonate only, the PH will not be high enough to fully convert everything, some harmalas will remain in solution and give it a yellow tinge, the amount is negligeable but I like to add few drops of NaOH solution to fully eliminate the yellow color. when you add the NaOH drop by drop and observe closely you will not see harmalas crashing out anymore but you will see the color change where the drop hits, you then mix a bit and add another drop and observe, repeat until the color stops changing. it can still be a bit yellow because of impurities so you should rely more on the color change.

I added a photo showing the water nearly colorless in the final basification step and after a couple water washes

have you seen the holy mountain? I love all the films by Alejandro Jodorowsky.

 

[aethereon]

Dang, I've never made it to colorless water. What the frick have i been consuming this whole time I guess some salty impure "rue-y" harmalas. I also did smoalk the salt form a bit too, thankfully not too much. Was mostly eating them and sublingualizing but yeah sheesh that taste left something to be desired.

I'll stop taking shortcuts now as well, a little bit of info/insight goes a long way...

I haven't seen anything by Alejandro Jodorowsky but I will definitely be checking him out now

Big Thanks Sakkadelic Hope you enjoy this AetherCookie

 

[Sakkadelic]

I'll dip it in milky harmala waters :b

A single basification + water washes or manske on rue tea is plenty good already but i like doing all the extra steps, it's fun since i don't struggle with filtration and i use simple coffee filters.

 

[isntme]

making the rue tea with whole seeds is also less messy and reduces the sludge and other contaminants.

would this reduce the extracted amount? perhaps boiling it longer to counter-act? I like the idea of letting it boil/sit longer and not have to filter so much.
I used my aeropress in combination with a box column drill (using the chuck to press) with good success for the DMT extraction. The point is that with vacuum you get less pressure (1 atmosphere) than with pressing. But still, it is some work to be done.

The freeze precipitation step (I had it from the maxIon tek; put the tea in the fridge for 12h) produced a good amount of stuff settling at the bottom (I used my large pipette to pipette the solution).

And how about storage? Any different than with DMT (i use Zinc de-oxy and silica gel, store it it the fridge for what needs to be accessible and freezer for the long term storage)?
Would one store the manske result (step 10 of tao tek) and then process further only smaller amounts? How fast does freebase degrade?

And a last one:
defatting with naphta is not necessary (vovin tek step 4) or may it even harm?

 

[Sakkadelic]

would this reduce the extracted amount? perhaps boiling it longer to counter-act? I like the idea of letting it boil/sit longer and not have to filter so much.
I used my aeropress in combination with a box column drill (using the chuck to press) with good success for the DMT extraction. The point is that with vacuum you get less pressure (1 atmosphere) than with pressing. But still, it is some work to be done.

The freeze precipitation step (I had it from the maxIon tek; put the tea in the fridge for 12h) produced a good amount of stuff settling at the bottom (I used my large pipette to pipette the solution).

And how about storage? Any different than with DMT (i use Zinc de-oxy and silica gel, store it it the fridge for what needs to be accessible and freezer for the long term storage)?
Would one store the manske result (step 10 of tao tek) and then process further only smaller amounts? How fast does freebase degrade?

And a last one:
defatting with naphta is not necessary (vovin tek step 4) or may it even harm?

I always got around 6% yield in freebase which is on the higher end of what is reported from rue extractions. and yes longer boils will ensure all harmala alkaloids are extracted. you can always keep the seeds and do more boils later. pressing the liquid out of the seeds between boils is maybe not necessary but it reduces the number of boils needed.

freeze precip? i haven't heard of that for harmala extraction. but yeah resting the tea in the fridge for a day and then discarding the stuff that settles at the bottom makes the filtering easier and results in cleaner product.

the harmala.hcl salt resulting from manske is very stable and preferred for long term storage. the freebase is more prone to degradation but I didn't have problems storing it in a air tight jar in a drawer.

yeah defatting is unnecessary, I never encountered any fats or oils with rue.

the difference with dmt extraction is that harmala freebase freely settles at the bottom so it can be easily retrieved by decanting the liquid and cleaned with water washes. dmt freebase is suspended in solution so a solvent is needed to pull it out.

 

[aethereon]

would this reduce the extracted amount? perhaps boiling it longer to counter-act? I like the idea of letting it boil/sit longer and not have to filter so much.
I used my aeropress in combination with a box column drill (using the chuck to press) with good success for the DMT extraction. The point is that with vacuum you get less pressure (1 atmosphere) than with pressing. But still, it is some work to be done.

Actually, recently with my latest extraction using the manske tek/tao of rue, just tried using the whole seeds. I went ahead and did multiple 'boils' of the seeds, more than reccomended, 4x if i remember. So there was a lot of liquid to filter and further reduce. However, my yield didn't seem to be as good; around 10g, but I had used a slightly larger amount of seeds to begin with than i normally use to get this amount... So while 'most' of the alkaloids may be on the outside of the seeds, it seems like there is still a significant portion on the inside.

Also, since I had such a large volume of liquid that was reduced, my resulting crystals were quite reddish. I basically stopped after the second manske but I have had other extractions that produced yellow(er) crystals as soon as the first manske was done. Not sure what exactly the red color means , maybe it's even a good thing. I do plan to redissolve and basify at a later point but I remember expecting a bigger yield given how much rue I used and how much I had boiled the (whole) seeds. For sure the filtering is way easier. However, maybe in the process of the extreme filtering with using ground seeds, some more of the impurities are taken out before even getting to the manske-ing?

I think if you have the time and patience and materials it is better to grind the seeds from my experience, but maybe the 'payoff' isn't worth it because you'll be using way more filter papers/cotton balls/coffee filters and for most people rue seems to be relatively inexpensive. Not to mention the time invested in said filtering.

The tao of rue also says to collect the filters/cotton balls etc and do another acid extraction on them, but I found that my yield from doing this extra work was minimal. As well It seems like all the sludge/dust sitting in the filters once again was a total pain to filter out after boiling them so for me I haven't seen much incentive in saving the filters/cotton balls. I wish I had taken a picture of my crazy collection though after doing one complete tao of rue, it seemed a bit excessive how much filter media it took. Of course with the ground seeds, less so with the whole seeds.

Also since I am using so many cotton balls I opted for organic cotton. I used to think organic cotton cloth was for 'crazy people' but looked into it and I guess cotton is one of the most heavily sprayed with pesticides crops there is. Maybe something to consider for those doing the tao of rue.

 

[isntme]

Thanks for your report.
I was thinking about using the same liquid and do 3 or so boil, freeze, boil cycles.
This should break up the cells and seeds without producing to much fine dust.

Yes, rue is at least for me far more accessible. I plan to go with a small aount of the available batch (50g), such that i can test different approaches if necessary.

 

[Sakkadelic]

An easy way to reduce the liquid volume is a base step, base with NaOH, let settle and decant the liquid, a couple water washes help clean things up, then acidify and add water to get an appropriate volume.

ime you need 5-6 boils + pressing the liquid out of the seeds between boils to get everything out. Freeze/thaw cycles before or inbetween boils helps. 5 mins microwave boils is the fastest approach but there's a risk of overflowing and dealling with scorching hot jars.

50g is a perfect amount to work with imo. The seeds swell and becomes bulky when working with bigger amounts. It should net you 3g freebase or 3.5g HCl salt.

The most critical part of a rue extraction to me is preparing the tea.

 

[isntme]

you need 5-6 boils + pressing the liquid out

So I was thinking of 3 cycles with the same liquid (sequezing/ working the seeds) and doing 3 pulls in total (as tao tek suggests), so 3x3 boils actually.
You refer to 5-6 boils with fresh liquid, right?

My thought is that the problem seems not the solubility (would require more fresh liquid) but to get the alkaloids out of the cells, but I might be wrong here...

 

[Sakkadelic]

So I was thinking of 3 cycles with the same liquid (sequezing/ working the seeds) and doing 3 pulls in total (as tao tek suggests), so 3x3 boils actually.
You refer to 5-6 boils with fresh liquid, right?

My thought is that the problem seems not the solubility (would require more fresh liquid) but to get the alkaloids out of the cells, but I might be wrong here...

yeah just enough to cover the seeds and account for evaporation. then pressing the water out of the seeds and boiling again with fresh water.

yes you're right, you need pressure to get it out effectively when working with whole seeds. the difference is that you are doing the squeezing steps separately from boiling while I'm alternating between the two.