I think that's exactly what @_Trip_ is saying. I was thoroughly satisfied with the results of harmala extractions without using Manske.
Manske precipitation is still a fun thing to do if you like growing beautiful, sparkly golden crystals, however!
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Purification after manske
- Thread starter Loveall
- Start date
Manske precipitation is still a fun thing to do if you like growing beautiful, sparkly golden crystals, however!
Kalitechnik
Esteemed member
Thanx. Time for my first harmala extract then soon 
Yeah as per post the NMR and HPLC tests are there. I too have been happy with this simple process and remember colour doesn't necessarily equate to purity. It can be a very fine min percentage of impurities that can throw out the colour.
Kalitechnik
Esteemed member
So what do you use for basyfing?
I strated my extraction and i wonder.... that typical NaOH that i usually use for dmt extraction is not a good idea here.
what would be better? i believe that something that is food grade? can you guide me in this step please.
Varallo
Chiaroscuro
In my experience ammonia is the best base since the excess wil vaporize upon drying and therefore leaves no residual base. It is as simple as to base with ammonia filter out the freebase and then wash with some water to remove most of the ammonia and then dry. If you have a Buchner filter with vacuum pump it’s even better.
Kalitechnik
Esteemed member
Hey guys regarding amonia, are we talking about Ammonium Bicarbonate ? I am going to buy it.
Also i wanted ask you for one thing. As i started doing my extraction i have noticed that filtering is rather pain in the ass.
One thing in the "no manske" technique was described is that we dont even need a filtering, and simply doing the settle/pour of method.
So my aproach was that after making a tea i did few of those, than i lye for first base, when it settled i decanted water from top and simply put some water with citric to make an acid stage.
and this liquid i poured through a coffe filter and i notice it is way easier then then trying to filter the base layer, get the freebase dry it scrape from a filter etc....
so i came up with this way of doing it:
1. Make tea - settle - decant
2. Base it - settle - decant
3. Acidify - filter
repeat 2 and 3 untill water gets clear (it became quite clear after 3rd cycle)
and than basify with ammonia for the last cycle, settle, pour of and collect all teh freebase on teh evaporation dish, warm it, evaporate and collect.
what are your thoughts on this please and what are you experiences?
thanks for your inputs it helps me a lot on my first extraction, i am very happy with it and i think it deserves a good tek and detailed description.
Also i wanted ask you for one thing. As i started doing my extraction i have noticed that filtering is rather pain in the ass.
One thing in the "no manske" technique was described is that we dont even need a filtering, and simply doing the settle/pour of method.
So my aproach was that after making a tea i did few of those, than i lye for first base, when it settled i decanted water from top and simply put some water with citric to make an acid stage.
and this liquid i poured through a coffe filter and i notice it is way easier then then trying to filter the base layer, get the freebase dry it scrape from a filter etc....
so i came up with this way of doing it:
1. Make tea - settle - decant
2. Base it - settle - decant
3. Acidify - filter
repeat 2 and 3 untill water gets clear (it became quite clear after 3rd cycle)
and than basify with ammonia for the last cycle, settle, pour of and collect all teh freebase on teh evaporation dish, warm it, evaporate and collect.
what are your thoughts on this please and what are you experiences?
thanks for your inputs it helps me a lot on my first extraction, i am very happy with it and i think it deserves a good tek and detailed description.
Varallo
Chiaroscuro
No ammonia is ammonium hydroxide solution in water, 5 % should be fine, and is available as household ammonia.
Hence the Buchner filter
This is the way to go, don’t use the settled stuff from step one but use the tea, and then from step two keep and use the freebase settlement.
I prefer to have at least one manske in the process after you lose all the plant material, mostly because the beauty of it.
I like to wash between the freebase and drying, it will reduce the smell from the ammonia and does not affect the yield. Citric acid is good to use but acidic acid is a good option to and might be more economical.
Take care
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Kalitechnik
Esteemed member
OK. Got it. Will go for it than. Maybe i will get 25%. I have a very good vendor for all kind of chemicals BTW.
I started to look around for some of that stuff.
Looks like i will give the manske thing a try one day.
Can you please explain a bit how do you do the washing part?
And i belive you meant ACETIC (not acidic) acid, right? And if i may ask why do you prefer it over the citric? And if there is any preference for the best acid?
As i told you i have a very good source of all kind of pure lab grade chemicals here where i am and prices are also very friendly.
Varallo
Chiaroscuro
Use proper PPE and use it in a well ventilated environment.
I can definitely recommend
After basing with ammonia just decant away from the freebase, then add some water, wait and then decant, you could repeat this if necessary. And yes Acetic I like it because it’s easier to use and is something that you have in the kitchen.
Kalitechnik
Esteemed member
Ok. Got it. Thanx. I will stick to citric acid since still i have loads of it.
And last question for now, once i will get a buchner filter, filtration gets easier.
And what about filtering through active charcoal? Does this makes sense? I read in origanal post of the "no manske" method, that he used some charcoal for filtration and the product was pure white after it. Whats your thought about it?
Bear in mind that you can produce ammonia from any ammonium salt, by mixing it with any strong base, but this requires a certain level of chemical know-how in order to perform safely (such as correctly setting up and operating the gas generation and absorption apparatus). So, again, I'm saying that it can be done, not that you should try it. If you can buy ammonia solution easily, there's not really any point in doing this unless you were wanting to hone your general chemistry skills. Producing and absorbing gases is quite a useful trick but also requires a solid understanding of the relevant safety protocols.
A further advantage being that it does evaporate relatively easily, with the corresponding disadvantage that it can stink a bit if you're boiling large amounts or higher concentrations of it.
Try it if you have it - add just enough that the colour has disappeared. Adding too much charcoal will reduce your yield as it is not selective. I would love to see you get white crystals this way. It can be difficult to filter off the small particles, so the lab trick is to use a layer of diatomaceous earth (sold for lab use as "Celite") in your filter funnel.
Kalitechnik
Esteemed member
I am performing the last step. Basified with amonia, and now washing, and decanting....
But something came to my mind, as i can see that the water i pour off my basified solution is glowing under the sun rays... So i belive (actualy i am quite sure)
that i am loosing some at this process...
and what i am thinking is if i am changing the PH with adding water, is this not like some separation of harmine and harmaline might happend, and that i am pouring some that is present in different PH? (i read that changing PH to some figures can make separation of harmine/harmaline).
So if this decanting/washing/neutralizing process is not creating any losses?
Varallo
Chiaroscuro
It does create a tiny loss because some of the harmalas dissolve or mix depending upon the Ph of the water used, this should though be a minimal loss, what you could do is evaporate the water for the sake of knowing how much the loss is or measure the Ph and if sufficiently high just let it settle for a few days. The glowing under UV light is not necessarily an a good indicator for the amount that is in solution because only a fraction is needed for this effect to occur.
Maybe I should mention that the amount of water used for the washing is minimal and only enough to remove the ammonia from the freebase, it doesn’t take much to do that.
Great job though and good to see your progress on your extraction.
Maybe I should mention that the amount of water used for the washing is minimal and only enough to remove the ammonia from the freebase, it doesn’t take much to do that.
Great job though and good to see your progress on your extraction.
Kalitechnik
Esteemed member
Ah. OK. So i think i overdid it. I mean i read in the original post that its good to neutralize the solution till PH8.... And as i thought it would need some "flushes".
So lets say i am using a 1L container for that, and after last amonia basing, when i poured of the liquid i think i washed it like 5 times, adding water waiting to settle/decant - repeat.
So you say, that mostlikely one time would be enough?
Varallo
Chiaroscuro
I would use approximately 100 ml for removing most of the ammonia from 50 grams of harmalas in a Buchner filter setup, just sprinkle the filtrate with a lab squeeze bottle.
I’m really sorry for not being more specific on the procedure before, I do think that if you have kept the water from your washing you will have no problem recovering the harmalas.
I’m really sorry for not being more specific on the procedure before, I do think that if you have kept the water from your washing you will have no problem recovering the harmalas.
Kalitechnik
Esteemed member
No worries. The loss is very minimal, and that was my first try, and i am just learning. And being very gratefull for all the help and tips from you guys here.
I am just ordering the buchner filter setup, and in some time i will be doing another extraction, so possibly we might be more specific... I really would like to share and document it, and make some easy description for the newcomers like me, since looks like that is a different approach to harmala extraction, then those who are well documented, and still some mentions grinding seeds, and all that filterings etc.... this aproach is way simplier, and as you said possibly being equipped with buchner filter that will became way way easier and faster.
Even dissolved CO2 is acidic enough to start dissolving a trace of alkaloids, principally harmaline as the more basic of the two (discounting THH for the moment).
I would say that it's the traces of ammonium salt - mostly ammonium acetate - that will be removed. Ammonia itself will simply evaporate, whereas ammonium acetate would hang around being hygroscopic, which is potentially annoying. A small hygroscopic film on the outside of the crystals would hang onto other impurities, and probably encourages oxidation too.
Kalitechnik
Esteemed member
Ok guys. Thank you so much for your assistance.
Proudly present my first ever harmala extract.
Nearly 3.5g from 100g of rue seeds.
See you in my next thread, where i will like to take things deeper.
Hopefully with your kind help.
Hats of fellow travelers.
Proudly present my first ever harmala extract.
Nearly 3.5g from 100g of rue seeds.
See you in my next thread, where i will like to take things deeper.
Hopefully with your kind help.
Hats of fellow travelers.
while vaping and eating dmt off course