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Cold Manske Options
 
ShadedSelf
#1 Posted : 6/18/2022 2:00:31 PM

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In my journey towards trying to understand/optimize manske Ive found that the recrystalization step by heating up the solution and letting it reach room temperature slowly seems to be unnecessary.

Adding NaCl to a harmalas β‰ˆ50% saturated room temp solution will precipitate, seemingly clean, bright yellow small needles of supposedly only harmine and harmaline.
This needles are big enough to stay on a 7-10 micron paper filter, and take a few seconds/minutes to form, rather than hours.
Instead of adding salt as a % of the solutions volume, you can add NaCl untill everything becomes clouded with needles, filter and add a bit more to push any remaining alkaloids out. Though 10 to 15 % seems to be a good starting point.

In my experience doing the manske step heating up the solution ends up with the big HCL needles full of brown/orange stuff the first cycle or two, and they only get golden towards the 3rd cycle.

This is also the time that Ive got the most out of a manske, 3.8% from the seeds, around 54% of the full spectrum extract compared to 45% following VDS ratios, I fell like there is still room for improvement.

Unless Im missing something I dont see the reason to recrystalize the harmala HCL needles.

Ive attached a picture of both the hot and cold manske from the same parent solution.
ShadedSelf attached the following image(s):
manske0.png (4,544kb) downloaded 221 time(s).
 

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downwardsfromzero
#2 Posted : 6/18/2022 9:23:36 PM

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Do you mean you're adding NaCl as a solid? Or as a concentrated solution?

Avoiding heating and cooling is if course desirable in terms of energy efficiency at the very least. Do you have any figures for yield or purity for comparing the hot Manske with the cold variety?




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ShadedSelf
#3 Posted : 6/18/2022 10:49:53 PM

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As a solid, I have NaCl in "flakes" or crystals, forgot to mention that, but that might be a part of it since it makes the salt dissolve somewhat slowly possibly giving more time for the needles to grow beyond tiny dust particles.

I did not compare yields beyond previous extraction numbers, I was admittedly too tired from the whole extraction process to add any extra steps Big grin
Also, the "spent" solution for both manskes looked identical.

Comparing yield should be easy, not sure how to compare purity.
My assumption is that cold manske needles look a lot brigther and golden from the beginning since other impurities dont have time attach themselves to the them, but upon filtering and redissolving both leave some brownish residue behind.
 
ShadedSelf
#4 Posted : 7/13/2022 10:48:26 PM

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Method:

1 Gram of Rue Extract is dissolved in 40ml of 8% acetic acid.
40ml of water and 14.4 grams (18% of the total volume) of NaCl are added to the solution.
This is similar to adding a fully saturated Harmala and a fully saturated NaCl solution of the same volume together.
Another sample is made with the same parameters.

The first sample is stirred, small yellow crystals start to form, then is left to sit for a few minutes and filtered.
The second one is stirred, heated in the microwave until everything dissolves and left to cool down slowly for 13 hours.

This might have been a bit too concentrated as needles seemed to have little room to grow.

Both samples were filtered, redissolved, based and weighted.


Yield:

The room temp crystalized manske sample weighted to 0.618mg, almost 62% yield.
The heated up manske crystalization sample weigthed to 0.620mg, 62% yield.


Purity:

Not sure how to test this one.

For some reason hot manske HCL needles look more brown, at least the first cycles, there is also way more sediment that doesnt dissolve back and stays on the filter, perhaps the heat could be degrading some of the vinegar??
Though once dried the brown color seems to disappear.

Hot manske HCL needles seem to hold less water once filtered and dry faster, this might mean slightly less salt contamination on the final product.

 
Loveall
#5 Posted : 7/15/2022 3:11:23 AM

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What happens to the filtered cold manske if you let it is it for a while? Wonder if other stuff precipitates with time.

What is 1g of "rue extract"? Is it precipitated free base?
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ShadedSelf
#6 Posted : 7/15/2022 10:36:30 AM

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Ive let both spent solutions sit for days after filtering, nothing crashes out, Ive also put the cold manske filtered solution in the freezer to see what happens, a tiny amount of small dustlike yellow particles precipitated, I asssume a bit of the remaining Harmine/DHH, probably too fast of a temperature drop and little amount of Harmalas to create any needles.

It was freebase "full spectrum rue extract", not sure what to call it, what you end up with after and couple of A/B, so there should be some other harmalas like harmalol, harmol and perhaps some quinazolines in there.

I dont think there is much difference between both manskes, as far as I can tell there is a balance between NaCl concentration, Harmala concentration and temperature, at the end of both manskes all three variables are the same.
 
Quetzal7
#7 Posted : 7/15/2022 8:49:36 PM

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Thanks for the idea ! When one work with 1kg of rue, this could save the painful process of trial error to hit the right spot for crystalisation (last time i had to re'dilute like 4 times, re-adjust the salt ... And heating it up everytime in beetween... plus risking to break my glass jars by pouring boiling water in it ... and making a mega mess all the time. )
I see here 1g for 40ml... i will take note of that ; i always mess up so much that i don't know anymore what's my ratios... but the ratio of harmal to water is as critical as the ratio of salt !
 
 
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