Limonene separated into 2 distinct layers, what to do?

[tango]

I don't remember this happening the first time around, but now my limonene separated as you can see in the first picture. Upon filtering it through a 103 qualitative paper, I can tell that there's no solids in the bottom layer.

Because the dark layer is very oily I figured I'd just go ahead and mix it all with the fumaric acid water, thinking that the oily stuff would separate anyway. It didn't happen; all I got was 2 layers: the limonene and the water with the oily stuff. Since it's been sitting in the funnel for a few hours, I doubt that further separation will occur any time soon. Also, the water I recovered is significantly more than the water with fumaric acid I used.

So now I'm evaporating the water from the brownish homogeneous solution, is that the right thing to do?
Thanks

ps. Is the use of swim, swiy etc really necessary?

 

[endlessness]

Is it possible the bottom layer was just a bit of the mimosa solution that got carried across (maybe as tiny suspended particles/?). I dont think you should keep that layer for the fumarate salting. Maybe if that happens again do a sodium carb wash on your limo and see if this layer will basically mix with the sodium carb solution (meaning it was indeed polar impurities, which is what it seems to be, hence why didnt separate frm the fumaric salting).

I would say the best for you to do now is to redissolve the fumarate salting in warm water, re-base and re-extract.

Good luck, tell us how it goes

 

[tango]

Thanks, now I'm (impatiently) waiting for the water to evap and I can already tell that whatever's left, it will be very sticky. I forgot to mention in my previous post that I used amor fati's method, which involves soaking the mimosa in a bit of vinegar at the very beginning, and then, later on, adding some water (with the lime). Now if acidic water does not mix well with the limonene, shouldn't we expect to have two separate layer in the mimosa solution, with the water+vinegar+whatever else got dissolved at the bottom?

During my first extraction I used the 'percolator', and the mimosa paste was still very wet when discarded;I believe the device works better with shredded/home pulverized material, as the powdered mimosa tends to clog it very quickly. The second time around, I got frustrated with the percolator and used vacuum filtration, first with qualitative fast and then with qualitative slow paper. That left the paste dry and powdery and, probably, extracted more of the oily solution.

As far as dealing with my current mix, do I need to wash the fumarates (I'm pretty sure there's excess fumaric acid too as, although I like the idea of using molar ratios, I doubt that my equipment allows for proper measurements; which is why this time I just used lots of acid and decanted, but that's not overly precise either) before freebasing or will the freebasing get rid of everything that should not be in the final product? I don't have the space for any creative setups and left alone, the evaporation takes forever :roll: I need to get a dehydrator !

 

[endlessness]

yeah the limonene should separate to the top but depending how well you mixed the whole thing and how fast you pulled it, it could be that there were some tiny droplets of the acqueous layer floating around that hadnt settled yet and you pulled before it had properly separated.

I never used amorfati or similar dry extraction methods do.

As for washiing the fumarates, yeah you can def do that. You can wash with IPA/Acetone (or recrystallize in them), if you want to use the fumarates, but if you're freebasing it wont really be an issue. Check BLAB tek or the "fumarates to freebase" wiki page for instructions on how to crystallize dmt freebase out of water when converting to freebase.

In fact you could even do this before waiting for the fumarate to fully dry.. Have it dissolved in a bit of warm water, add sodium carbonate saturated solution and let it in the frige for a couple of days.

good luck!

 

[tango]

That's exactly what I was wondering about: why is there a need to wait for the fumarates to dry if you're gonna be adding water again when freebasing ?! If you have the fumarates+ water+excess fumaric acid, adding sodium carbonate should neutralize the excess fumaric acid and separate the spice from the fumarates, right? Then one can just decant the solution to get rid of the sediment and wait for the spice to precipitate.

I was wondering: is there was a thread with all the chemical reactions this community has managed to figure out, the conditions for the reaction to happen (temperature, solubility etc), the catalysts, and so on? I'm very thankful for teks such as the "10 minute freebasing", but I feel that some steps/quantity are rather random (especially the quantities). If the authors gave a reason for the procedures/chosen quantities, that would be great. Besides, when working with such small quantities and cheap Chinese scales, it's a lot more convenient to use as much solute as you want and then remove the excess (as long as you know you need a saturated solution) than trying to combine say .450g solute with 7.5 ml solution etc.

As far as getting several layers in the initial phase, where you're collecting the limonene, it seems to me that if one follows amor fati's tek, it would be more surprising to get just one homogeneous mix. When water+fumaric acid is added to limonene, it's assumed that the spice will migrate from the limonene to the acidic water. However, the first thing you do according to the above mentioned tek is you moist the bark with vinegar, then add the calcium hydroxide and moist again with water. After that you add plenty of limonene, but the water and vinegar are already there. Now if the spice would rather be in the acidic water than limonene, shouldn't we expect it to migrate to the water/vinegar mix as soon as it's extracted from the mimosa and into the limonene? As in bark -> limonene -> water/vinegar mix.

Because if that happened, then by the time one adds the water+fumaric acid, there's not much left in the limonene, as the alkaloids are already concentrated in that water/vinegar solution.

I know this is long, but this separation of the solution extracted from the mimosa is not mentioned in the tek, and it seems that theoretically it needs to happen. Furthermore, that small layer at the bottom may contain more actives than all the limonene, so I figured I'd check to see what others think about this

ps. I keep seeing all these questions about how purify your spice. I'm talking here about eliminating the other stuff that's extracted with the spice, not about removing solvent residue. My question is: is there any issue with smoking plant oils, provided you can vaporize them? People smoke all kinds of herbs, and I'm assuming a lot more than the targeted active compounds go into that smoke. And yeah, I surely don't care what color my spice is.

 

[endlessness]

That's exactly what I was wondering about: why is there a need to wait for the fumarates to dry if you're gonna be adding water again when freebasing ?! If you have the fumarates+ water+excess fumaric acid, adding sodium carbonate should neutralize the excess fumaric acid and separate the spice from the fumarates, right? Then one can just decant the solution to get rid of the sediment and wait for the spice to precipitate.

I was wondering: is there was a thread with all the chemical reactions this community has managed to figure out, the conditions for the reaction to happen (temperature, solubility etc), the catalysts, and so on? I'm very thankful for teks such as the "10 minute freebasing", but I feel that some steps/quantity are rather random (especially the quantities). If the authors gave a reason for the procedures/chosen quantities, that would be great. Besides, when working with such small quantities and cheap Chinese scales, it's a lot more convenient to use as much solute as you want and then remove the excess (as long as you know you need a saturated solution) than trying to combine say .450g solute with 7.5 ml solution etc.

As far as getting several layers in the initial phase, where you're collecting the limonene, it seems to me that if one follows amor fati's tek, it would be more surprising to get just one homogeneous mix. When water+fumaric acid is added to limonene, it's assumed that the spice will migrate from the limonene to the acidic water. However, the first thing you do according to the above mentioned tek is you moist the bark with vinegar, then add the calcium hydroxide and moist again with water. After that you add plenty of limonene, but the water and vinegar are already there. Now if the spice would rather be in the acidic water than limonene, shouldn't we expect it to migrate to the water/vinegar mix as soon as it's extracted from the mimosa and into the limonene? As in bark -> limonene -> water/vinegar mix.

Because if that happened, then by the time one adds the water+fumaric acid, there's not much left in the limonene, as the alkaloids are already concentrated in that water/vinegar solution.

I know this is long, but this separation of the solution extracted from the mimosa is not mentioned in the tek, and it seems that theoretically it needs to happen. Furthermore, that small layer at the bottom may contain more actives than all the limonene, so I figured I'd check to see what others think about this

ps. I keep seeing all these questions about how purify your spice. I'm talking here about eliminating the other stuff that's extracted with the spice, not about removing solvent residue. My question is: is there any issue with smoking plant oils, provided you can vaporize them? People smoke all kinds of herbs, and I'm assuming a lot more than the targeted active compounds go into that smoke. And yeah, I surely don't care what color my spice is.

Yes adding a sodium carb solution before drying it should work perfectly. Check the BLAB in the wiki for instructions on converting fumarates to freebase with slow water crystallzation method, and just adapt as if you have dissolved your fumarate in water. Just dont have it with too much water otherwise it might interfere with crystallization (though im speaking theoretically, it could be that even with a lot of water it will still work fine, but having it more concentrated before adding the sodium carb is a good idea).

As for the information on reactions, im sure you've been reading the WIKI? There is a lot of information there, some different teks explain better than others. Regarding "conditions for reactions", would you be more specific? Is there any specific reaction you are wondering about?

For example the freebasing of a substance is dependant on the pKa and pH of the solution. All the info on pKa is in this WIKI page, and you can easily calculate what pH is necessary to freebase a substance by using this calculator.

One thing to notice though, is that, first of all, regarding the 10 mins conversion, is that the person who did that (Ice House) found out by accident, and he is no chemist, hence why no accurate measurement. It was very nice of him to share the results with us. Other teks might be more specific. Also, a lot of people dont give specific measurements but more general ideas because these extractions are very forgiving. Its kind of like cooking, if youre making a bread with cheese, do you need specific measurement of how much cheese and bread? If you use waaaaay too much cheese its probably gonna fall all over and not really work, and if you use too little its gonna be pretty boring eating pure bread, but there is a quite big range there where it will be fine.

Lastly, regarding plant oils and when its ok to smoke dmt, check this thread out and see if it helps. A bit of plant oils shouldnt be a problem, youre right!

 

[tango]

Thanks, that's a great page. I didn't really know much about the wiki... I believe the teks are listed there, but other than that, I used to just search the main site and then use google.