First rue extraction: What do I do with the filtered Manske solution? (with PICS).

[PresentlyAbsent]

Hello!

I followed the Tao of Rue Extraction and successfully extracted harmala alkaloids. My main question is:
What do I do with the filtered solution that is a product of the Manske steps? The guide says to keep this solution and "reduce it some more to 'push' any stray alkaloids out"

I reduced the solution by a lot (perhaps too much) and a lot of salt precipitated. This makes sense as it was roughly 10 g NaCl per 100 mL. But it's not clear what to do after its reduced. My intuition tells me to redissolve it in hot water and base it with sodium carb. But would I then need to wash the solution to get rid of the excess salt?

Anyway, my extraction was successful. I got about 1 g of harmalas from 75 g of seeds (roughly 1% to 1.5% yield). This is quite a bit less than the 3-5% yield I expected. The low yield is probably due to some harmalas still in the Manske filtered solution. I also expected a low yield since it's my first (complete) extraction and I spilled a bit and made a number of unnecessary container transfers.

I took some pictures to document the extraction. The step numbers match the steps in the ToRE.

• Step 1, 2, 3, & 4
I started with 75 g of rue seeds from. I did not grind the seeds. I tried grinding before, it made filtering a nightmare. I think I could handle it a second time around now that I have more experience filtering, but I've elsewhere on the Nexus that it doesn't make a significant difference. When filtering the solid seeds from the tea I used a course stainless steel (SS) mesh, a fine SS mesh, and lastly paper coffee filters. I skipped the cotton balls in the funnel filtering method. I think my fine metal mesh is roughly the same pore size as the cotton. I'm not sure on the mesh size - but the fine mesh is rather soft and flexible.
IMG: This is the tea after it had been filtered through coffee filters. This is 5 seperate 40 min boils .

• Step 5: Base
In a seperate bowl, I combined room-temp water with sodium carb. I made the sodium carb by backing sodium bicarb (baking soda) in an oven at 400°F for 2 hours. Internet sources said 200°F for an hour works, but I wanted to be sure it all converted. I poured this solution in the tea and an immediate color change from yellowish-brown to yellowish-cream occured, as expected.
IMG: This is after adding sodium carb solution to the tea
About 24 hours later, the mixture settled. I decanted the liquid and filtered the solids with coffee filters.
IMG: Solids after adding base for the first time.
IMG: I redissolved the solution in a hot 3:1 mixture of water:vinegar and filtered again.

• Step 6: Manske
I followed the "recommended" Manske procedure. That is, mix 10 g of salt per 100 mL solution. I had about 90 mL so I added 9 grams to the hot solution. I let the solution cool slowly to room temp, then left in the fridge over night. The crystals stopped growing after around 5 hours, but I let it go over night.
IMG: Crystals in the jar.
IMG: After decanting.

• Setp 7: Filter
IMG: After filering the first Manske.
IMG: Close up shot of crystals on coffee filter

• Step 8,9:
I redissolved the crystals in a minimum amount of water and added another 9 g of NaCl for my 90 mL. However, when I added the salt yellow crystals started forming immediately. I believe this is because the solution was warm and not hot. After it cooled completely and I filtered, the crystals were very thin and very yellow (butterscotch as some say). I was a little disappointed because I expected them to be even redder than from the first Manske.
IMG: Crystals filtered from my second Manske step spread out on a coffee filter.
I decided to re-Manske. This time I made sure the solution was piping hot and I also dissolved the crystals in about 1.5 times more water/vinegar to allow room for the crystals to grow.
IMG:Crystals in a jar after my third Manske attempt. Very pretty.
IMG: The same crystals filtered and layed out on the filter paper.

The guide calls for the Basing/Manske-ing steps to be repeated at least one more time to increase purity. I was more concerned about completing the extraction that I decided to skip straight to the final basing (also I was pretty exhausted by this time -- this was day 4 of the extraction).

After basing with sodium carb (I decided not to seperate harmine and harmaline), I washed and dried the alkaloids and got a nice looking tan powder.
IMG: Final extracted harmala alkaloids.

I couldn't wait so I vaped about 25 mg of the harmalas in my GVG. I found I had to remove the diffuser to get enough heat on them. About 5 min later I vaped ~20 mg of DMT. I did not break through but I felt the calming of the harmalas and the experience definitely lasted longer. I very excited to try pharmahuasca. While vaping DMT is incredible, it is so short and sometimes holding my breath on the third or fourth toke is hard. Breathing just feels so amazing!

Anyway, I just wanted to say I'm very grateful for the Nexus as it has been a tremendous resource.

 

[wearepeople]

Awesome writeup PresentlyAbsent!

This is a stellar example of how to write up an extraction process and ask questions!

And awesome pics! Those needle photos are pretty!

In regards to your main question: You can take the filtered solution (and yes, your intuition was correct) and base it to recover more alks. Once the alks have settled to the bottom, decant the liquid off the top.

Essentially, you can take any of the "waste" liquids and also the used filters, combine them all, acidify, base, and recover more alks. If you're going to use the filters, I'd stay away from the ones that are full of the dark, sticky sludge.

As far as I know, the purity of alks from such a method might be lower but preliminary evidence shows that they'll be nearly devoid of Quinazolines (vasicine, deoxyvasicine, vascinone). Mind you, this is not fact, simply preliminary evidence.

Adding a base to the `spent` solution post-manske will still yield a significant amount of harmalas with smaller (but possibly significant) amounts of other alkaloids.

Check out this post and the rest of the thread for more information.

Once you've recovered from the "waste" of the extraction, clean 'em up as you did in the preliminary extraction. If you do recover from the "wastes", please be sure to update this thread with results! I'd love to see how it goes for you.

Or if you're exhausted from extracting harmalas, just call it quits and enjoy!
wap

 

[Jees]

... But it's not clear what to do after its reduced. My intuition tells me to redissolve it in hot water and base it with sodium carb. But would I then need to wash the solution to get rid of the excess salt?...

As an alternative to reducing of the remaining acid-salty solution: If you base the total remaining solution, and filter the settled precipitations out, all your salt is gone. Redissolve this matter in your filter in a new lower amount of volume, to manske again, at higher concentration this time due the lower volume.

 

[PresentlyAbsent]

Thanks, wearepeople! I'm glad you liked the write up.

I will base the solution and see what precipitates. I'll post an update in a day or two.
That link was VERY helpful! Was that a stickied post? There are a number of "epic" posts on the Nexus, but some of them are hard to find.

Jees: You're right. In hindsight it is obvious that there is no need to reduce the Manske solution. The Tao of Rue Extraction says to reduce it, but perhaps they were working with larger volumes of liquid.

 

[wearepeople]

Nope, its not a Sticky. Its still in progress.

Yeah, sometimes the Epic threads are a bit buried. Collecting the gems and putting them in a thread is a good resource to create for everyone.

For example, I created a "map thread" for the FASA process.

Its a wonderful thing for someone to do when first going through a new process because its fresh in your mind and you have an idea where other beginners would have questions and where they could find the answers.

Taking this idea a step further, like Entropymancer does, pulling the main quotes out of the Gem threads and compiling them is wonderful. Here's an Entropymancer example also about FASA.


~wap~

 

[MelCat]

Great work and awesome write-up PresentlyAbsent!

I voted for your promotion. You seem sincere in your learning and grateful for the chance to be here.

Good luck on your future journeys!

 

[Jees]

What do I do with the filtered Manske solution?

...Jees: You're right. In hindsight it is obvious that there is no need to reduce the Manske solution...

Logic says so, but ahummm.. just tried and it failed majestically in precipating + filtering, lol.

First pic, the harvest of 50 gr treated rue seeds, 3.6 grams of harmalaHCL dried manske product (good for 3 gr freebase, so 6% yield --> wearing happy face).

Then based the manske liquid to pH 11.5 and got a nice white forming, after 24 hours settling the layer at the bottom is like in the 2nd picture (the volume is like 1 liter). One could swear to be able to filter this out, but the white just fell trough the coffee filter, it was not really solids but more like a waxy white layer. The only thing that was able is to decant the translucent layer off, which comes down to a volume reducing of some kind. But filtering = nope. If one wishes to reduce volume further, then real reducing by boiling is still necessary I guess, which will happen later given some spare time.

 

[sjaman]

The harmala HCL looks kind of weird too, should be darker and pinkish red imo. Dissolved in water it looks like cognac.

What I noticed on the tao of rue tek is that the first base really should be done with naoh, because of all the particles (i guess) in the solution. Else the ph is not going to be high enough with just sc.

When you do a manske direct after the boiling, and just filter with a normal coffee filter you do not need noah for basing and can just use sc, but the yield is a little lower.

 

[Jees]

The harmala HCL looks kind of weird too, should be darker and pinkish red imo

It's not weird, just more pure . My style is to A/B as much as needed to obtain a very glass crystal clear yellow solution before the manske step taking place. Each acid state gets filtered to the bone, each time catching dirt. In the last base-step the decanted layer was almost clear as water.

What I noticed on the tao of rue tek is that the first base really should be done with naoh, because of all the particles (i guess) in the solution. Else the ph is not going to be high enough with just sc.

For the result posted, muriatic was used for the soaking/boiling, for A/B's phosphoric and Naoh, pH wavering between 3 and 12. Manske step was with phosphoric pH 3 to 4.

 

[sjaman]

The harmala HCL looks kind of weird too, should be darker and pinkish red imo

It's not weird, just more pure .

You are probably right, i never tried to manske pure harmalas, maybe it will look the same as yours

 

[Jees]

The white balance in the pic is a bit of-target, in real it is more deep warm yellow.
These pics are from a previous session, the yellow is more true here.

 

[sjaman]

looks beautiful!

 

[PresentlyAbsent]

Jees, thanks for the pics! It's really nice to see that.

I based and filtered my manske solution and got abou 75 mg of a brown powder. It was noticeablly darker than the harmalas extracted from standard procedure. This is what I expected after reading this thread.

The picture attached is the 75 mg in a baggie.

What I noticed on the tao of rue tek is that the first base really should be done with naoh, because of all the particles (i guess) in the solution. Else the ph is not going to be high enough with just sc.

I just got some NaOH (lye) and I am going to use that instead of sodium carb for my next rue extraction. I will deviate a little from the Tao of Rue Extraction by not Manske-ing. I'm not (currently) pregnant, so I'm not worried about the aborticant properties of the vascicine and the vasicinone. Like last time, I also won't seperate the harmine from the harmaline. I'm interested in the rue "full spectrum" as opposed to experimenting with individual molecules. This should also produce a higher overall yield. I'm excited to try again, but it probably won't be for about a month.

 

[Jees]

You have something to start with :thumb_up:

So I tried to re-basify that captured manske liquid after harvesting the harmalaHCL, giving me that waxy layer I told of:

After failed filtering of that layer, I recovered something like 50% of that layer, let is settle for few days in it's own pH 11.5 water, it crushed onto itself making a thinner layer and forming some nice white needle crystals. But that was not the goal, so decanted all the base-watery top layer off to get a smallest volume possible (200ml). Not wanted to reduce volume further by cooking. If this wasn't going to work, then pfff
Made it acid pH 3.5, heating it, adding 20 gr salt, let it cool and wait for needles forming, nothing. In this experiment I got really nothing out of re-basifying the manske liquid in a higher concentration/ lower volume. Some tiny flakes floating and little dust on the bottom, but no nice yellow harmala needles of any kind.

After days in the fridge in 200 ml: nothing: