I've made a concoction of rue, basified it to pH 10.8 with sodium carb, decanted off the green liquid and kept the precipitated alks.
Now I'd like to make sure there are no more alks in the green (basic) liquid (which BTW has now gone down to pH 9.6 - presumably due to the freebase alks having been removed). Can I Manske it directly to push out the stray alks, without bringing the pH down? If I need to decrease the pH first, how low does it need to be for Manske to work? And is it worth it?
My thinking is, there are no more freebase alks in the green soup, but there may still be harmaline salts that didn't convert to freebase due to the pH not being high enough. Manske works on salts, so it could work?
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shouldn't it be easier to raise PH of your green solution to 11,5 or so and then precipitate your alks ?
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I don't have lye. As I was approaching the 10.8 it was becoming exponentially difficult to raise the pH and the amount of sod carb that took me like from 7 to 9 only raised the pH from 10.7 to 10.8. I feel I'd need a ton of it to get to 11.
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I've been trying for quite some time to see a detailed explanation of a Manske, and I keep coming up unsatisfied. In 'the tao', https://wiki.dmt-nexus.m...traction#Step_6_-_Manske - is this quote: Quote:
"Step 6 - Manske
Once you have redissolved your alkaloids in a minimal amount of fresh, hot vinegar and then filtered the solution, it's time to perform the manske.
There are three ways you can perform the manske.
The first and the "official" way is:
Recommended
Take a note of how many ml's you have and add 10 grams salt per 100ml solution. Make sure your solution is hot before you add the salt, otherwise the harmalas might fall out too soon. Allow to cool slowly.
The second way by Phlux-:
Prettier Crystals
Take note of how many ml's you have and saturate the same amount of fresh distilled water with salt. Add them together and allow to cool slowly. If the first solution wasn't overly saturated with alks, you should get needles that are similar to what's pictured to the right. This seems to work better with an excess of water/vinegar to allow the crystals more room to grow.
The third way:
Completely saturate the solution with salt and allow to cool.
Not Recommended for Final Manske due to the higher chance of more salt contamination. It's better to use one of the above methods, preferably Phlux's on the final manske and push any remaining alks out by reducing the solution further after you filter the harmala hcl.
Step 7 - Filter"
In the above snippet, it leaves me hanging at 'allow to cool slowly'. This thread - https://www.dmt-nexus.me...aspx?g=posts&t=73792 calls out a dead link - I really have tried to find something in fuller detail, but I'm coming up empty. I'm not looking for a detailed, scientific explanation, I'm merely a kitchen diddler with no chemistry background. So, if anyone could point me at a slightly fuller explanation, I'd appreciate it very much. Thanks. " Enjoy every sandwich." - Warren Zevon
"No, they never did turn me into a toad." - Pete (O Brother, Where Art Thou?)
"Are you a time traveller?" "No, I think I'm more of a time prisoner." - Nadia Vulvokov (Russian Doll)
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@jagube i'd acidify, reduce and manske @sunnyside check this picture and this. When it's hot they are soluble and when it cools they crash out, the slowly is just so bigger crystals form Sakkadelic attached the following image(s):  20180426_190116.png (1,256kb) downloaded 65 time(s)."Is this the end of our adventure? Nothing has an end. We came in search of the secret of immortality, to be like gods, and here we are... mortals, more human than ever. If we have not obtained immortality, at least we have obtained reality. We began in a fairytale and we came to life! But is this life reality? We are images, dreams, photographs. We must not stay here! Prisoners! We shall break the illusion. This is Maya. Goodbye to the holy mountain. Real life awaits us." ~ Alejandro Jodorowsky
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You cannot do manske on basic solution. Manske precipitates HCl salts, which means you need protons. Manske works by shifting equilibrium. It is called Le Chatelier's principle. Adding an excess of chloride ions to an acidic solution of alkaloids, the system will compensate to try and get rid of some of those ions by precipitating the less soluble protonated harmala chloride salts. --- didn't read your whole post, if the pH is not too high and there are still harmala salts, manske can work. Keep in mind manske does not precipitate to completion nearly as much as raising to the pH to 10 does. Manske might get you some harmaline at pH 8-8.5, but you already pushed it to 10 so I wouldnt expect much of anything. Manske is an excellent way to get high purity harmalas as a step before basification, sacrificing a bit of yield (not much, maybe 5-10%). Expect nothing, Receive everything.
"Experiment and extrapolation is the only means the organic chemists (humans) currrently have - in contrast to "God" (and possibly R. B. Woodward). "
He alone sees truly who sees the Absolute the same in every creature...seeing the same Absolute everywhere, he does not harm himself or others. - The Bhagavad Gita
"The most beautiful thing we can experience, is the mysterious. The source of all true art and science."
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Yes as already said here, your best bet is to re-acidify, reduce, re-base, filter, dissolve in fresh water, then Manske.
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Jagube wrote:I've made a concoction of rue, basified it to pH 10.8 with sodium carb, decanted off the green liquid and kept the precipitated alks.
Now I'd like to make sure there are no more alks in the green (basic) liquid (which BTW has now gone down to pH 9.6 - presumably due to the freebase alks having been removed). Can I Manske it directly to push out the stray alks, without bringing the pH down? If I need to decrease the pH first, how low does it need to be for Manske to work? And is it worth it?
My thinking is, there are no more freebase alks in the green soup, but there may still be harmaline salts that didn't convert to freebase due to the pH not being high enough. Manske works on salts, so it could work? There are still alkaloids in the basic water. Harmalol will be there. I think others too since they still have some minor solubility in a base. Turn on a UV light and reduce the pH of the filtered basic water, it will go from red to dense green. There's the harmamol we usually trow away. Unfortunately it is difficult to get harmalol out since it does not precipitate or seem. At a pH of around 9 it will move into the right olvents (Chloroform/DCM, and if you salt to form layers and push zwitterions out IPA seems to also work-but then you need a strategy to remove the salt from the IPA, I have not tested xylene but that may be worth a try). Also, harmalol can degrade, I think due to it's -OH group so a strategy to preserve it is also needed (maybe shoot for a vitamin C or other antioidant acid salt). In many ways harmalol and psylocin present the same type of extraction difficulties. If anyone is interested in getting at the harmalol we can discuss moar.
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Loveall wrote:There are still alkaloids in the basic water. Harmalol will be there. I think others too since they still have some minor solubility in a base. Thanks, I'm only interested in harmine and harmaline here and I'm going to Manske the collected precipitate anyway. My only worry is the basic water may still contain some harmaline. Mindlusion wrote:Manske might get you some harmaline at pH 8-8.5, but you already pushed it to 10 so I wouldnt expect much of anything. I hope there is not much harmaline in there as that would mean I can discard the green soup. But how do I find out if that's the case? blue.magic wrote:Yes as already said here, your best bet is to re-acidify, reduce, re-base, filter, dissolve in fresh water, then Manske. Hmm, if I just reduce the basic soup, will more alks crash out? I didn't mention I've already re-acidified and re-based the soup once, albeit without a reduction (but with filtering). After the first basification it had lots of particles in suspension and I feared some alks might have gotten stuck in those. So after collecting the first precipitate I proceeded to re-acidify, filter and re-base, and collected some more alks.
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To add to what has been said, harmaline/harmine HCl turns out to have low solubility when cold which we also use to our advantage.
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