• Members of the previous forum can retrieve their temporary password here, (login and check your PM).

Rue harmalas solubility in vinegar?

Migrated topic.
q21q21

q21q21

SWIM
OG Pioneer
SWIM has found that when drying and scraping rue harmalas (freebased and precipitated with sodium carbonate) there is usually a lot of gunk still stuck in the filter.

This time SWIM just soaked the coffee filters in vinegar and made sure everything was dissolved while he stopped whenever the vinegar stopped changing color.

So now he was a brown-red solution of unknown concentration, while bioessaying could give him a general idea, he figured might as well see if someone has the exact information before doing that.

Thanks
 
The harmalas, at least harmine and harmaline is VERY soluble in vinegar. I'd say 100mg harmine should be soluble in less than 1 ml of 35% vinegar.

The harmalas are bitter, that is one way I notice if there are actives left.
 
SWIM is getting a PH meter soon (at least he hopes soon) and he'll try the seperation tek.

Thanks though.
 
So when one performs a manske of any sort, then, the Vinegar is best to be boiled off, especially if one uses a lot. Otherwise, the harmalas could be trapped in the Vinegar right? I am asking because I just took freebase cappi alklaloids (fresh) and maybe used the wrong order: I put the filter paper directly into the 100ml 10g salt solution and added more vinegar as was coming up to boil realized that (me-dummy) salt was not going to help the wet freebase harmalas dissolve-- then dissolved slowly but dissolved. Anyway, after cooling, NO Precipiattion of Harmalas; and the solution smells a lot of Vinegar. So it is funny to have found this thread.... I'm thinking the residual Vinegar may hold the harmalas that the Sodium Chloride is supposed to push out...
 
plumsmooth said:
So when one performs a manske of any sort, then, the Vinegar is best to be boiled off, especially if one uses a lot. Otherwise, the harmalas could be trapped in the Vinegar right? I am asking because I just took freebase cappi alklaloids (fresh) and maybe used the wrong order: I put the filter paper directly into the 100ml 10g salt solution and added more vinegar as was coming up to boil realized that (me-dummy) salt was not going to help the wet freebase harmalas dissolve-- then dissolved slowly but dissolved. Anyway, after cooling, NO Precipiattion of Harmalas; and the solution smells a lot of Vinegar. So it is funny to have found this thread.... I'm thinking the residual Vinegar may hold the harmalas that the Sodium Chloride is supposed to push out...
Click to expand...


I believe the salt converts the harmalas into an hcl which is insoluble in a saturated saline solution so they should not be trapped in the salt saturated vinegar.

My friend has done it with straight 5% vinegar and it worked.
 
Original Manske calls for 100g Salt per Liter 1000ml of Water.

Yet the actual solubility of salt in water is 36g per 100ml,

that's three times as much...

What's the deal here:

Should one use a saturated salt solution, or use the original Manske recipe?

I almost made a separate thread; I have never heard anyone discuss this differential...
 
but notice thats the solubility of salt in pure water, not in rue tea...

anyways, no need to be exact.. I just keep the tea boiling in a pot, keep adding salt and stiring until no more dissolves, then into a container and to the fridge...
 
endlessness said:
but notice thats the solubility of salt in pure water, not in rue tea...

anyways, no need to be exact.. I just keep the tea boiling in a pot, keep adding salt and stiring until no more dissolves, then into a container and to the fridge...
Click to expand...

Same here. My friend started off trying to weigh out the salt needed but could never replicate to get an exact amount. So now he just gets it to a med boil and start pouring in salt until it doesn't all mix in. He pours it into a 1000ml beaker leaving behind the undissolved salt and lets it sit out for a few hours so he can watch the magic. Then puts it in the freezer and goes to sleep.
 
I just keep the tea boiling in a pot, keep adding salt and stiring until no more dissolves, then into a container and to the fridge.
Click to expand...

Well I used to think that would lead to excessive salt in the the precipitates...


until I read that water only holds about 4 more grams salt per ml when boiling...

However, the differential of 40 grams while boiling a liter is too close for me to chance having a tbl of salt ending up in my mush.

I guess if you know your recipe that's different...
 
excess salt is no problem at all because you should anyways redissolve your precipitated alkaloids in fresh warm water and then add sodium carbonate to freebase them, and any excess salt will stay in the water and not precipitate
 
Well I was working with Caapi and I wanted to finish with hydrochlorides.
I really like the needles and thought the hydrochlorides would be the best finish.
I had about 1 gram of wet freebase on a 7cm 103 filter paper and threw it into the glass teapot in 10G/100ml solution and added some Vinegar.
Realizing that I should have re-dissolved the freebase in vinegar first before adding it to the water/salt, I added a little more vinegar.
When it was dissolved and hot I filtered and set to precipitate in Fridge.

Nothing came...

Thinking the excess remaining vinegar was holding the alkaloids back,
I re-boiled attempting to rid the leftover vinegar in solution.

Set agin in fridge, salt ratio same, at 10g/100ml.

Finally gave up, rebasified...

Fortunately salt and sodium carbonate don't seem to mind each other.

I have recovered my alkaloids in solution and will filter tomorrow.

Wondering if Manske with Caapi is really worth the bother?

But knowledgeable ones: IS there a convenient way to convert the Caapi Harmalas back to dried salts for dosing after basing...

Am I just being to attached to keeping them in that form?
 
endlessness said:
excess salt is no problem at all because you should anyways redissolve your precipitated alkaloids in fresh warm water and then add sodium carbonate to freebase them, and any excess salt will stay in the water and not precipitate
Click to expand...
Why do manske, if you are doing sodium carbonate precipitation later on? Any benefits to doing a manske first?
 
for rue yeah, two major benefits: firstly, manske eliminates unwanted alkaloids like vasicine/vasicinone, which would be present if one only bases it... Also, successive manske precipitations clean the harmalas and you dont lose any, while base precipitation might make you lose some harmaline with every precipitation because it is slightly water soluble as a base. So I usually make a few more manskes and only a couple of base precips to get the harmalas really pure and not lose so much yield
 
I think an interesting experiment would be to separately re-Manske 2 grams of Harmaloids, one with 10g/100ml and one with 20g/100ml Salt and see if the later brings back more. Otherwise I would conclude that there is a large window with the salt and the presense, even at half saturation in enough to flush out the harmaloids.

Now as far as the Caapi harmaloids I can't come up with a reason why they didn't precipitate with Manske at all, other than that the concentration of them wasn't enough with the given Manske salt solution.

One more thing, sorry to run this into the ground, but is there a reliable tech for simply converting the freebase Caapi harmalas back to salt form without Salting them out Manske style.
 
Back
Top Bottom