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washing harmine/harmaline hcl in water

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jamie

jamie

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Okay so I have some relativly pure harmine/harmaline crystals from 200g of harmala seeds..I am wondering if I can simply dissolve the harmine and harmaline hcl in hot water and then stick the solution in the fridge and wait for the harmalas to drop back out? Both harmine and harmaline hcl are not super soluble in cold water right? So they should drop out eventaully? I want to end up with the smallest ammount of salt contamination as possible..

The product I have now is the end result of just blending the seeds with water and vinegar at high speed..then boiling them 3 times..decanting and filtering..and then repeated manske over and over until long terminated needle point amber xtals were dropping out. I did this because I do not like the A/B convertion after the first manske. I have done manske-A/B-manske in the past, and personally I think that the A/B step leads to a loss in yields. I got really pure product but not alot of it. I dont know why..I always loose yields that way and am confident that it is not just impurities. I am much happier with the time consuming manske over and over..but I want to rextal from just water as my last step..

I also prefer harmine and harmaline hcl and do not care for the freebase.
 
they should be VERY soluble in water, maybe even in cold temperatures, unless you add some salt to that water. Try it out though, at most you'll just have to re-heat, add excess salt and let it precipitate again.

maybe your suppose loss of yield when a/bing is at least partly of impurities? Also notice the HCl molecule adds weight, plus some salt contamination even if minor. But yeah its possible there is small loss of harmaline in each base precip, but if you do it just once at least, you'll clean from a lot of contamination and not lose so much.

Also you can do side-by-side tests to see if you really lose anything (or you can re-acidify and then re-salt the basd water to retrieve alkaloids that you think are left over, if there are any)
 
So I dissolved them in hot water..and stuck them in the fridge...once cool nothing was precipping..so I heated the solution back up and added some salt saturated water..still nothing was dropping out really as it usually happens quite quickly..stuck it in the fridge and came back after an hour and this is what it looks like...
 

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This was from only repeated manske salts only..I really love manske teks even though alot of people here seem to like A/B teks more these days..I love watching large hcl needles form on the jar and line the bottom..I wonder if I dissolve them in hot water and then just freeze the water and thaw it out if that will precip cleaner xtals without having to use any salt..
 
Nice :) How much cleaner it is now than before, if at all?

I doubt freezing and thawing would work. If there's too much salt maybe water would form slurry and not even freeze? Or if it freezes, maybe it still doesnt really precipitate, or maybe it redissolves quickly as it thaws? I dont know, try it out and let us know, I would just guess it wouldnt work.

I think the best way is to use minimal amount of salt and very slow cooling (leave it standing in water bath till water goes cold, even better if water bath has some insulation to keep temperature for long, and only when its at room temp, put in the fridge). You can always add more salt to the water after filtering to make sure all harmala hcl has precipitated (though this will obviously lead to more salt impurities, so you keep them separate).
 
well it should be somewhat cleaner because the water is still holding that brownish amber tint..every time I remanske the water keeps that amber color so that must be impurities..the crystals are growing in larger and nicer formed clumps this time also..

I will experiment with different approaches for a water re-xtal to see if it is possible..

Also..what color should pure hcl harmine/harmaline xtals be? All the other times I saw pictures of pure hcl salts they were always amber and never white..mine are always amber as well..I have never gotten white hcl salts, but if I convert them to freebase they are white..convert them back though they are amber again so I am assuming amber is just the color they take on as a salt?
 
fractal enchantment said:
well it should be somewhat cleaner because the water is still holding that brownish amber tint..every time I remanske the water keeps that amber color so that must be impurities..the crystals are growing in larger and nicer formed clumps this time also..

I will experiment with different approaches for a water re-xtal to see if it is possible..

Also..what color should pure hcl harmine/harmaline xtals be? All the other times I saw pictures of pure hcl salts they were always amber and never white..mine are always amber as well..I have never gotten white hcl salts, but if I convert them to freebase they are white..convert them back though they are amber again so I am assuming amber is just the color they take on as a salt?
Click to expand...


This is perfect. You have slowly cooled the solution and and added salt. Now your getting really nice crystal formation. You need to vacuum filter the solution leaving your product behind. Even a hand vacuum pump will work..but you may need a few filters. If you don't have access to a pump then just follow the standard Gibran tek from here....decant...add water...decant...add water....decant...dry.

BTW I can't express the importance of at least a hand vacuum pump for final product work. It's the best way for 'home gamers' to separate their product from the toxic solution it is in. IMHO. Plus they are pretty damn cheap.

BTW. Those crystal are looking good. That looks like so much more than 200mgs to me!


Edit: Pure crystals are off white.
Edit again.....my bad. Pure free base crystal are off white.

Peace.
 
okay..so I filtered the water out and collected the harmine and harmaline hcl from the filter(I dont have vaccume filter but I wish) and let it dry..I then dissolved it in a very small ammount of hot water..enough for it to dissolve. Then I stuck this into the fridge once it cooled a bit. Very little was precipping out..not really much at all..so I stuck it into the freezer..20 minutes later there are nice xtals dropping out. They were a bit smaller in formation than before but a lighter tint of amber-more translucent. I stuck it back into the freezer for about 15 minutes..more xtals are dropping out..and the jar is all frosty inside..so I think maybe I can just put it into the fridge now..

15 minute later and TONS of xtals are dropping out..but the solution has also frozen a bit for some reason-it was not frozen in the freezer..but anyway I can see tons of xtals that have dropped out..it is full of nice translucent amber crystal formations..and these are precipped from just water, no salt. I put it back into the fridge for now..

I am unsure as to what is going to happen now..if it warms the slightest back into a liquid solution the xtals will either redissolve or stay crystalized out..I think the key is to find the perfect temperate just before the solution begins to freeze but cold enough to precip hcl salts from a small amount of water alone. This should take care of any excess salt contamination.

Edit..even after being left a room temp for 10 minutes it was a semi frozen slushy thing full of xtals..so I concluded it needed a bit more water..I added a small ammout of spring water and stirred it. The xtals did not seem to dissolve but it did turn it back into a lquid solution with the crystals suspended in it..I stuck it back into the fridge to see if it all drops out and precips a bit more maybe without turning back into a slushy.
 
It worked..here is a picture of what the water precipitation looks like..
 

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When I used to toy with beta-carbolines I liked to rinse the HCl crystals with cold saturated NaCl solutions. There is some loss, but it removes a lot of the reddish grunge. This also enables a person to do a Manske in very small amounts of water.

edit -
Next time, it might be best to use boiling water if you can handle it safely. Obviously there is dangers associated with boiling water :). Not saying that for you jamie or any of the pro's but we don't want an accident.
 
You can do this with harmala fumarate. Its much less soluble in water than the hcl, and it will precipitate out of cold water very well without salt. You just have to titrate it carefully to avoid excess fumaric acid. It would be interesting to see how malic acid and tartaric acid salts precipitate, as those acids are much more soluble in water than fumaric, so if you overshoot how much acid to use, it won't precipitate out when cooled like fumaric acid will.

Hcl's are pretty soluble even in cold/concentrated solutions with out added salt to precipitate them though. at least thats been my experience with them.

I say if you want hcl's, and have muratic acid, just dissolve the freebase in dilute hcl water and evap. Then if you want pretty xtyals, dissolve it in a minimal amount of boiling distilled water, and add nacl saturated distilled water at 1/2 the volume of the water you used to dissolve the hcl's.
 
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