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simple titration, and dual solvent crystalization
- Thread starter dg
- Start date
damiana
Cosmic Dragon
Hmm, the mescaline sulfate doesn't want to precipitate out, I'm guessing this is because swim never boiled down the water before adding acetone. Oh well. SWIM will have to evaporate that.
SWIMs second pull evaporated. 200mg of mescaline sulfate was collected, 100mg was eaten by SWIM just a bit ago. SWIM has only had mescaline acetate, which was never pure. SWIM thinks that maybe mescaline acetate is too acidic, pulling extra stuff with the mescaline. Not sure really, SWIM just wants pure mescaline, clean and simple.
SWIMs second pull evaporated. 200mg of mescaline sulfate was collected, 100mg was eaten by SWIM just a bit ago. SWIM has only had mescaline acetate, which was never pure. SWIM thinks that maybe mescaline acetate is too acidic, pulling extra stuff with the mescaline. Not sure really, SWIM just wants pure mescaline, clean and simple.
yes, you might notice i dont use CAPS much, reducing solovent volume via boiling is not for everyone.
sparkless hot plate/boiling chips/stirrer and fume hood are advised
eventually the acetone will evap, and then you can reduce the water via boiling..
sparkless hot plate/boiling chips/stirrer and fume hood are advised
eventually the acetone will evap, and then you can reduce the water via boiling..
narmz
Rising Star
benzyme said:
What sort of device is that? SWIM would love to test this out, sulfates seem really hard to filter and take a long time to settle, maybe this'd help. And just to make sure SWIM understands correctly, you got a jar with 60%acetone/40%water inside of a beaker with water/ice in it to cool down the temp, and then some sort of device that reaches in to the 60/40 mix and emits ultrasonic vibrations intermittently? Can you do a comparison of typical recrystallization to that which is ultrasound assisted? Does it settle faster?
Touche Guevara
Rising Star
The HCL salt is insoluble in IPA, isn't it?
Touche Guevara
Rising Star
So if I understand correctly, it's possible to dissolve impure mesc HCL in water, add some volume in acetone, and freeze precip? Is there a ballpark rule for the water:acetone ratio? I ask because Phlux- posted a tek some time ago for removing cellulose (iirc) that was performed similarly. Dissolving the mesc HCL in a small amount of water and adding a copious amount of acetone will precip inactives. Perhaps these precipitates could be filtered and then the mix frozen to precip the actives?
w0mbat
Rising Star
Touche Guevara said:
IIRC it actually is soluble in 99% IPA (that is, assuming my friend's home-made 99% IPA is actually 99%. There's no way to test). However, according to his tests, it the HCl salt is less soluble in 99% IPA than it is in water - therefore 99% IPA might be a better choice for dual-solvent re-x. I was hoping dg could comment on this.
Touche Guevara said:
I've heard someone say that this doesn't work well in practice. I think the person tried about 1 g of impure HCl salt, ~0.9 mL of distilled water, and 2 mL acetone. He also said that his results may have been poor because he did not wash his crude product before attempting re-x.
thought i'd add this for info's sake, this was a help thread given to a friend by me and others when his dual solvent crystallization stalled
Quote
i followed everything step by step, i did a third pull, and boiled it down after titration. it stopped reducing at 500ml. i added all my mesc xstals i needed cleanedand then I added 600ml of acetone and threw it in the freezer, it never got cloudy, theres no xstals on the bottom or anything. did i fuck up big time?
No, but you didn't reduce as much water as you should have, which is why nothing crashed out when you put it in the freezer.
Quote
did i use too much acetone? it stayed in the freezer last night, ive got it back in the freezer.
No, you didn't use too much acetone, mescaline sulphate is not soluble in acetone, the problem is that there is too much water in there, not too much acetone.
Quote
what can i do to get my xstals back? yesterday i had alot, then i tried to re-xstal and now i have none. I know its its there, but how do i get it out?
Remove the acetone, by setting up a warm water bath in a well ventilated space, and then placing the solution in a bowl placed in the warm water bath with constant stirring or else a boiling stone until there's no more smell of acetone. Once the solution warms up, it should start bubbling as the acetone will start boiling out.
Once the boiling stops, then all the acetone will have boiled out, and it will be safe to remove the bowl, and place it on top of a pan of boiling water to create a steam bath, make sure there's a gap between the bottom of the bowl and the top of the boiling water. Now keep heating it until the solution reduces.
Measure the temperature if you can. You'll see that as the acetone is boiling, the temperature of the solution would be around 56°C. Then when you place the bowl on the steam bath, the temperature of the solution will rise, if you have a fan placed to blow into the bowl, it will help reduce the solution quickly. And with a fan on it, the temperature would be around 80°C or so, because as the water evaporates it takes heat out of the solution, and the fan speeds up the evaporation of the water.
Eventually when you keep heating it, you'll notice that all of the sudden, the temperature of the water starts climbing again, if it goes over 100°C, then it's gone past the boiling point of the water, because the solution is super saturated. This is the point to remove the solution and allow it to cool to room temperature, and then add the acetone.
If you add acetone to superheated solutions (solutions above their boiling point) then the acetone can sink to the bottom and then superboil spraying the hot solution all over the room. This is why I suggest removing the acetone from the solution in a warm water bath first, before sticking the solution onto a steam bath. A pot of just boiled water works to make a warm water bath, and it's important that you do this in a well ventilated place.
Now in order to recrystallise mescaline sulphate, typically you'd add 5 mL warm water per gram of mescaline, and heat it and add a few drops of water at a time until all the mescaline has dissolved. Then you allow it to cool, and add acetone.
Mescaline sulphate is a good one, because it is much less soluble in cold water than mescaline hydrochloride is, so it's not so fussy about crashing out if there's still plenty of water in the solution. But in your case 500 mL water is way too much water for the amount of mescaline dissolved in it.
AND:
Quote: would it be safe to put the solution back on the hotplat and reduce it more? or is that way unsafe since acetone is highly flammable, its used as an octane booster ffs.
is it safe to try to reduce or evap or do i need to go ahead and filter it end quote:
No, don't stick acetone containing solutions on the hotplate, not unless you are doing this in a very well ventilated fume cupboard. Doing this in your kitchen with the window open is not good enough ventilation for using acetone on a hotplate, it's just not safe.
It is safe to remove the acetone by sticking the solution in a bowl and placing the bowl in a pot of just boiled water, then once the acetone has boiled out, the temperature of the solution will be over 56°C. You may need to swap the water for fresh just boiled water several times. But do it like that, rather then use an electric heat source near the acetone solution.
Also it can be dangerous to your yields to heat the mescaline sulphate in water solution directly on top of the hotplate. This is because once most of the water has been removed, the temperature will start climbing above 100°C, and get so hot, that if there's any excess sulphuric acid, it can destroy the mescaline.
So if you can measure the temperature of your hotplate and set it at a level that is around 100°C, then it's fine to use. Otherwise it's safer to reduce the mescaline sulphate solution by sticking it on a steambath. So if you can't monitor the temperature of your hotplate, it's safer to sticking a pan of boiling water on the hotplate, and stick a bowl full of the mescaline sulphate on the pan of boiling water, than it is to stick the container of mescaline sulphate solution, directly on the hotplate.
Steam bath's can heat above 100°C, as steam is hotter than boiling water, but they don't go up to levels hot enough to scorch the mescaline sulphate, like hotplates can. But still you should monitor the temperature of the solution, because it will let you know what's going on
and the end results: shiny white crystals
once i reduced down the solution far enough, the ratio didnt matter. the first time i tried, i didnt boil enough h2o out of the mesc solution. Acetone had nothing to do with the failure.
The 2nd time i boiled all the h20 out and when i added the ice cold acetone, the solution separated on its own and the crystals crashed out.
It was all about boiling ALL the h2o out of the mesc sulfate solution.
Maybe a 1 to 1 ratio of acetone water would be enough to crash out all the MS, but I added more to be safe.
Quote
i followed everything step by step, i did a third pull, and boiled it down after titration. it stopped reducing at 500ml. i added all my mesc xstals i needed cleanedand then I added 600ml of acetone and threw it in the freezer, it never got cloudy, theres no xstals on the bottom or anything. did i fuck up big time?
No, but you didn't reduce as much water as you should have, which is why nothing crashed out when you put it in the freezer.
Quote
did i use too much acetone? it stayed in the freezer last night, ive got it back in the freezer.
No, you didn't use too much acetone, mescaline sulphate is not soluble in acetone, the problem is that there is too much water in there, not too much acetone.
Quote
what can i do to get my xstals back? yesterday i had alot, then i tried to re-xstal and now i have none. I know its its there, but how do i get it out?
Remove the acetone, by setting up a warm water bath in a well ventilated space, and then placing the solution in a bowl placed in the warm water bath with constant stirring or else a boiling stone until there's no more smell of acetone. Once the solution warms up, it should start bubbling as the acetone will start boiling out.
Once the boiling stops, then all the acetone will have boiled out, and it will be safe to remove the bowl, and place it on top of a pan of boiling water to create a steam bath, make sure there's a gap between the bottom of the bowl and the top of the boiling water. Now keep heating it until the solution reduces.
Measure the temperature if you can. You'll see that as the acetone is boiling, the temperature of the solution would be around 56°C. Then when you place the bowl on the steam bath, the temperature of the solution will rise, if you have a fan placed to blow into the bowl, it will help reduce the solution quickly. And with a fan on it, the temperature would be around 80°C or so, because as the water evaporates it takes heat out of the solution, and the fan speeds up the evaporation of the water.
Eventually when you keep heating it, you'll notice that all of the sudden, the temperature of the water starts climbing again, if it goes over 100°C, then it's gone past the boiling point of the water, because the solution is super saturated. This is the point to remove the solution and allow it to cool to room temperature, and then add the acetone.
If you add acetone to superheated solutions (solutions above their boiling point) then the acetone can sink to the bottom and then superboil spraying the hot solution all over the room. This is why I suggest removing the acetone from the solution in a warm water bath first, before sticking the solution onto a steam bath. A pot of just boiled water works to make a warm water bath, and it's important that you do this in a well ventilated place.
Now in order to recrystallise mescaline sulphate, typically you'd add 5 mL warm water per gram of mescaline, and heat it and add a few drops of water at a time until all the mescaline has dissolved. Then you allow it to cool, and add acetone.
Mescaline sulphate is a good one, because it is much less soluble in cold water than mescaline hydrochloride is, so it's not so fussy about crashing out if there's still plenty of water in the solution. But in your case 500 mL water is way too much water for the amount of mescaline dissolved in it.
AND:
Quote: would it be safe to put the solution back on the hotplat and reduce it more? or is that way unsafe since acetone is highly flammable, its used as an octane booster ffs.
is it safe to try to reduce or evap or do i need to go ahead and filter it end quote:
No, don't stick acetone containing solutions on the hotplate, not unless you are doing this in a very well ventilated fume cupboard. Doing this in your kitchen with the window open is not good enough ventilation for using acetone on a hotplate, it's just not safe.
It is safe to remove the acetone by sticking the solution in a bowl and placing the bowl in a pot of just boiled water, then once the acetone has boiled out, the temperature of the solution will be over 56°C. You may need to swap the water for fresh just boiled water several times. But do it like that, rather then use an electric heat source near the acetone solution.
Also it can be dangerous to your yields to heat the mescaline sulphate in water solution directly on top of the hotplate. This is because once most of the water has been removed, the temperature will start climbing above 100°C, and get so hot, that if there's any excess sulphuric acid, it can destroy the mescaline.
So if you can measure the temperature of your hotplate and set it at a level that is around 100°C, then it's fine to use. Otherwise it's safer to reduce the mescaline sulphate solution by sticking it on a steambath. So if you can't monitor the temperature of your hotplate, it's safer to sticking a pan of boiling water on the hotplate, and stick a bowl full of the mescaline sulphate on the pan of boiling water, than it is to stick the container of mescaline sulphate solution, directly on the hotplate.
Steam bath's can heat above 100°C, as steam is hotter than boiling water, but they don't go up to levels hot enough to scorch the mescaline sulphate, like hotplates can. But still you should monitor the temperature of the solution, because it will let you know what's going on
and the end results: shiny white crystals
once i reduced down the solution far enough, the ratio didnt matter. the first time i tried, i didnt boil enough h2o out of the mesc solution. Acetone had nothing to do with the failure.
The 2nd time i boiled all the h20 out and when i added the ice cold acetone, the solution separated on its own and the crystals crashed out.
It was all about boiling ALL the h2o out of the mesc sulfate solution.
Maybe a 1 to 1 ratio of acetone water would be enough to crash out all the MS, but I added more to be safe.
The little mouse
Rising Star
acetone is heavier than air, can a vent hood remove it? I boiled acetone a few times in my life.... super yucky!!!
The little mouse
Rising Star
lol, thats where i always did it!!! bad idea though
highRvibratoryfreq
Rising Star
What initial extraction tek do you use when you refer to foaf? Or better still which would people recommend if you wanted to process 1kg of cactus?
Help appreciated!
:thumb_up:
Help appreciated!
:thumb_up: