Sometimes the manske can get a bad rap, I really don't know why. I think it's easy, effective and awesome.
Who else loves the manske precipitation?
These greasy xtals were filtered in about 20 seconds. Salt residue is minor and cannot be detected by taste. They could be cleaned further for aesthetic reasons but should work just fine how they are.

Those are amazing!

The best I ever get out of Manske is brown crud that's always salt heavy. I usually do an A/B on it afterwords to get tan crud.

Very, very impressive.

I'd love to know how you get xtals like that.

Alzabo

Wow, really nice work...


Much Peace and Rainbows

Very nice! I too am curious how you separated the precipitates so cleanly from the supernatant. Looks like mostly harmine needles. Excellent work.
L

Here's my method. It still needs a lot of work. If you have any ideas, please do write them up.

200g rue seeds are ground.
Seed powder is put in a pot and covered with vinegar.
This mixture is simmered for a while.
The mixture is allowed to cool so that it does not hurt to touch.
The mixture is poured through a muslin cloth into a vessel.
The seed powder in the muslin cloth is squeezed dry.
The exhausted powder is set aside to be dealt with later...Perhaps I will use it as plant food for rue seedlings.
1L NaCl saturated solution is prepared with room temperature water.
A vessel is prepared with a marking at the 1L line. I put two pieces of duct tape on a 1gal jar, one piece marking the surface level of 1L and the other marking the meniscus level of 1L. Additionally, a rubber band was secured about the circumference of the jar for ez reading.
The rue water is mixed with the NaCl saturated water. In the newly prepared vessel.
The liquid in the vessel is heated until reduced near the 1L mark. For me, this meant putting the jar in a very large pot on top of a rag. This would have gone a lot quicker had I contrived to put the entire solution in a pot instead of a 1gal glass jar. Out of impatience, I removed the jar from the pot with upwards of 500mL liquid above the 1L mark.
The vessel is allowed to cool. I left it on a top shelf and forgot about it for 2 days.
Once cool, the mixture is swished about and poured through a gold filter. Red Xtals are collected in the filter, the liquid passes through easily. This is the part that took me all of 20 seconds.
The liquid can be added back into the vessel to allow for more xtals to precipitate.
The filter is turned upside down and smacked against the bottom of a new vessel to collect the captured xtals from the filter. This was actually a mistake, see the next step.
The filter is held over the xtal collection vessel and hot water is poured through it to dissolve any xtals that didn't get smacked out. Some solids and goos will remain in the filter. This material can be discarded.
More hot water is added to the xtals and the mixture is heated until all xtals present have dissolved. I added some isopropyl alcohol at this point. That was probably a mistake as the harmala xtals should be completely soluble in plain water. The addition of iso might cause more impurities to get dissolved. This is bad, see next step.
Some material will not dissolve even after heat and agitation is applied. This material is removed by sending the hot liquid through the gold filter again.
The liquid is poured into a dish and evaporated. I did this at room temperature for nice'n'spiky xtals but the same could be accomplished on a double boiler.
Alternately, don't evaporate the liquid and precede to step one for further purification.

Yield so far is 18g. That's out of 200g seeds and it looks as though I'll get another 2g out of the liquid in my 1gal jar that is slowly evaporating, towards the 1L mark, at room temperature. 20g out of 200g is 10%. Erowid lists 7% as high harmala content for rue. Assuming that my seeds are high yielding at 7% dry weight, that would mean my extract is only 70% pure. It seems worthwhile to repeat this process a few times in order to determine if I have super ultra active seeds or if the extract is really 30% or plus impurities.

As you can see, I already have many critiques for myself. I know there are a slew that I am not even considering. Any question? Hit me!
I'd really like to get this process streamlined as much as possible. It's already fairly quick to complete a single manske but if it were even easier, I'd do several of them every time just to get nice clear xtals -- a product that can be dosed with great accuracy.

Not to burst your bubble but, 7% is unheard of(never seen a yield from anyone that high with even close to tan). Not to mention you also have Chlorine being added to the molecular weight, so the Harmala HCl is going to weigh more than plain Harmala freebase. 3%-4% is much more common for purified extracts in my limited experience(or 1%-2% with worse techniques). Judging by the color of your extract alone, I'd recommend doing a few a/b's on it. Nice goopy crystals though .

Personally I find manskes more well suited for small volumes of water.

For example: 250mL(volume depends on how many grams of extract are being added of course) of boiling water get's almost saturated with NaCl(not completely saturated because then when it cools there is a lot of salt precipitate, look up the solubility data for water at 25*C and use that ratio). Then crude harmalas are dissolved in the solution. Stir while the solution is cooling to form a nice yellow precipitate, filter it into a coffee filter.

Then I've had some limited success with this but with the precipitate sitting in the coffee filter in a short spouted funnel, add nearly boiling hot water to it(as little water is possible, this is somewhat tricky). The harmalas will dissolve with stirring and go through the coffee filter and into the container below. As the water cools, some crystals will form. I'm sure this could be altered for better results .

edit- was the dish heated to drive off water? It looks like you have a ring of N-Oxide around the edges of it in the first picture.

Anyhow cool stuff nice post.

7% yeild on rue is not uncommon imo -

sorry - reread - manske done as above doesnt produce a pure product - only via addition of minimal salt water - just enough does one get absolute clear xtals
when i state yeild i always state freebase - as salt purity is down to tek and thus no indication

yeah I could def see that based on my experiences so far with rue tea. I was surprised at how potent even just 1 gram of rue is..def enough for me to trip mildly and need to go lay down.

None of the published literature I've seen puts the % alks to be that high...I've never encountered seeds that yielded that high when subjected to manske + a/b...Not saying you're wrong...more curious as to if there's anything behind anecdotal evidence to support calims of high yields. Some guy in another thread claimed to repeatedly yield 10-15% harmalas from rue, but he never answered any of the questions I asked re: method, purity, etc...

go wild extract kilos and see for youself - 10-15% sounds high but still even belevable - perhaps the alkaloid content directly relates to its potency as a dye.
its belevable that it may have, in some areas, undergone selective breeding to increase dye strength and thus making one requre less dye stock(quantity of seeds)
especially as the areas its traditionally from is dry and prone to drought - meaning less avaliable bio product.
just an idea - perhaps the ability to flouresce under uv increases the brighness or shinyness of the dyed object / carpet with map to the other worlds.

No offense phlux but 10-15% being believable? Are you serious? And what's the point of measuring the yield of an impure product? Are you joking? That's like buying a crate of oranges, including the weight of the crate as the weight of the oranges... Are we talking wet weights here or something?

I'd sure love for someone to come up with a technique for 7% purish(at least TAN colored). If you have one share it I'll test it this week with 200grams of rue. Though I'd rather not put my money on this because I've done pressure cooked extractions on completely powderized material(doubt a single cell wall remained after 30 minutes at 15 psi). Using minimal water(the freebases are slighlty but ignore-ably soluble in water) and extra care to pH ratios to stay where 99.9% of the calculated freebase microspecies of harmine & harmaline where viable, and got around 4%. The biggest losses in extractions from my experience is not being able to pull the goodies out of a/b goo(which can easily be remedied with probably with the loss of a few nanograms from the yield). The seeds I've seen just do not produce that much(ordered from 4 different vendors so far from india, to the U.S. resellers at different times of year).

Just don't believe it until I see it or it is documented. As stated above NONE of the scientific references mention a 10% let alone a 15% yield by weight. A 7% is certainly out of the norm.

Well also you need to add the hcl ion weight, did you calculate that?

I did read of 7% yields in some publications though, and also infundibulum mentioned to me he had similar yields even after purifying it. But I never read or heard of more than 7% from a trusted source. Personally my yields where more like 1-4% by doing manske+loads of A/Bs to get pure white harmalas, but for sure some was lost in the clean up steps.

I would guess there is some salt contamination there, as is normal with manske, as well as the HCl ion, just make some mole calculation.

Wow infund pulled off a 7%? I'd certainly love to see the technique he used? Link?

The biggest variable I can see is potency of seeds, and if there are seeds with 10%-15% then who is selling them? Or are they not available to the public and strictly used for the manufacture of dye-stuffs?

id say 5% is about average.
surely hcl - doesnt make up a large % of total salt weight on harmalas - usually it adds just a tiny fraction right ?(unlike the bulky fumaric acid)
nothing iv said holds water until i retry this whole thing but im out of a decent quanity of rue.
i guess i got about 20-30g to try again - this time il be thorough and record freebase amounts with pix of the entire process.
been long enough since i last manske'd

Burst away! I am a frothy-bubble-machine, so there are always more where that came from!

That's a good point about the harmala-hcl being heavier than harmala freebase.
Can anyone tell me in what ratio harmine and harmine combine with HCl?
What does the molecular EQ look like when the solution of harmala acetates is saturated with NaCl?
I am teh noob chemist trying to become an advanced beginner in this subject.

I'm a bit reluctant to do A/B cleanups because harmaline freebase is slightly soluble in alkaline water.
I'd much rather do repeated manskes to get a clean product then follow up with a set of base precips to seperate harmine and harmaline.


See the second to last step in my extraction log -- no heat was used. Perhaps the edges are N-Oxide but I don't think so because they taste and look the same to me. I think it's just a different crystal structure than elsewhere. There is however more oil residue around that ring because the oil was floating on the surface of the water and stuck to the edges of the dish as the water level reduced.

Once I finish getting everything out of this first manske, I'll proceed to clean up some of it. I'll be sad to lose the oils though because they actually give the product a rather nice flavor. -- still, after seeing this quote from phlux, I'm excited about growing extra large ultra pure xtals --

Thinking about dosing this, if I wanted to take the equivalent of 200mg freebase, assuming that the extract is 70% freebase by weight, i would need to take approximately 286mg.
On the other hand, if the seeds contained a more typical 5% harmaloids, then extract is only 50% pure and I should be taking 400mg extract to equal 200mg freebase.

Sanity check; is my reasoning sound?


I do not understand what you are saying here.
Will you please explain what you mean about minimal salt water.

Ok here's the calculation:

Harmine molecular weight: 212.25 g/mol
Harmaline molecular weight: 214.26 g/mol
HCL molecular weight: 36.46 g/mol

So making an average between both harmine harmaline (we dont know beforehand the ratio in your particular batch so lets just make half way) = 213.25

213.25 + HCl (36.46) = 249.71

so to find out the percentage that HCl represents in 249.71, one would divide 36.46 by 249.71 and multiply by 100, = 14.6 %

So reduce 14.6% of your yield to know your freebase harmala weight (this does not consider other impurities such as excess NaCl that precipitated together, which is probably present at least to a small degree)

(edit2: calculation is right yeah, the H is also there)

Beautiful, thank you endlessness.
I wasn't sure if the harmalas would combine with HCl in a 1:1 ratio or not. Now it is clear.
From there, I reckon that if the seeds yield 7% harmaloids in freebase form, then my extract would contain only 16% impurities as 14% of the weight is accounted for by the weight of one HCl per harmaloid freebase unit.
Ya reckon?

Edit: i see your edit and say that i just used 14% instead of 14.6%...sooooo I dunnae. I was wondering what happens to the H a well.

like 40% by volume of vinegar pulls of salt water