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How long does it take d-Limonene to evaporate?

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CosmicLion

CosmicLion

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SWIM was extracting from 225g of pink inner-bark MHRB. The bark is about 2 years old.

SWIM used much excess citric acid (300+ grams) to do 5 gallons of extract from MHRB using The Herbal Percolator. The solution was boiled down to about 2/3rds of a gallon.

SWIM added excess NaOH to heavily basify and counteract all the citric acid. The pH meter topped out around 12 and SWIM added a good amount of extra NaOH to make sure pH got driven closer to 14.

In total SWIM used about 1 liter of d-limonene to try and get out all the actives.

SWIM reports that after 36 hours the d-limonene has evaporated to a thick yellow goo that still seems relatively voluminous. The goo has started to form a very few chunky crystals in it.

Once the bulk of the d-limonene is evaporated, how long does it take to get the residual solvent out of the goo? Does it ultimately get thicker and more waxy?

Will evaporated d-limonene always leave a thick goo?

Should SWIM keep the fan on it or maybe try a desiccant chamber?
 
instead of evapping limonene, which is quite wasteful, I guess it would be more practical to, once basified and made pulls with limonene, mix limonene with vinegar.. this would make alkaloids migrate to vinegar.. then the limonene is separated (and can be reused), evap the vinegar down to get sticky dmt/jspice acetate.. then mix with sodium carbonate or similar and a little bit of water to make paste, mix mix, and this should turn it into freebase again.. then you can use alcohol or a much smaller amount of limonene to pick up the freebase, and then finally evaporate it to get freebase (though it would be not only dmt, but jungle spice also)..

this is all theoretical for SWIM so far because he will only be able to try this for first time in a couple of weeks, but it sounds more reasonable then evapping a whole liter of limonene.. Its possible that limonene leaves some residues, so thats why using a minimum amount of it as I described would probably make things easier as there would be fewer residues.

but now for SWIY I guess its maybe too late, a lot of limonene was evapped already.. though you could mix it again in vinegar (or any acidic solution, basically) and do as mentioned.

or try it out to just continue with fan or desiccant chamber and tell us the result :)

good luck!
 
Sounds like a great technique to try.

SWIM is unclear on the paste part.

If a sodium carbonate\spice paste is made, then mixed with alcohol, what happens to the sodium carbonate?

One believes the sodium carbonate does NOT dissolve well, if at all, into alcohol. It seems it may be hard to separate such a small amount of carbonate from the alcohol.

An experiment just showed SWIM that if water is heavily basified with NaOH that Iso Alcohol will separate like a solvent, forming a nice top layer.

Would it be better to take the acetate salts and mix with maybe 75-100ml of water, then basify using sodium carbonate?

Once a high pH of 10-12 is reached Iso Alcohol can be mixed in, separated, collected then evaporated for spice.

Is this along the lines of what you were saying, or did you have a particular logic in using the paste?
 
are you sure all the iso alcohol separated, or part of it only? maybe im mistaken but part of it would probably be mixed up in the water and only part on top, screwing your yields

when mixing the paste with alcohol or limonene and filtering, the sodium carbonate should stay behind, and they should only pick up the alkaloids.. The paste is made like this because then you would probably need less limonene than if you had to again make pulls from an acqueous solution, so the evaporation would be faster and have less residues.. and in the case of alcohol simply because it would work, because if its with water it would mix with the water instead so it would screw things up.

what we need now is some more chemically inclined people to confirm if limonene/alcohol would indeed leave everything except alkaloids behind, or if it could pick some of the stuff up.. I guess when one mixes sodium carbonate and dmt acetate it becomes sodium acetate + dmt freebase..

So now gotta check if sodium carbonate (if one used more of it than the amount of acetic ions in the dmt acetate so there is still some remains of it), and sodium acetate (in case this does form) are soluble at all in limonene or alcohol. Because otherwise then it would work as predicted, just picking up the alkaloids and leaving the rest behind, and one could use a minimal amount and get a reasonably pure product in the end
 
SWIM has Basic Water + Isopropyl Alcohol test results.

Thesis: Isopropyl alcohol will fully separate in a solution of water that is heavily basified.

Mixture: 400ml Water combined with 200ml 70% Isopropyl Alcohol

The amount of total pure alcohol was calculated.

460ml Water and 140ml Pure Isopropyl Alcohol were made into a solution.

Note: 1 Tablespoon NaOH = 13 grams

Test 1: 1 even tablespoon of Sodium Hydroxide (NaOH) was mixed into solution. No separation occurred.

Test 2: Another even tablespoon of NaOH was mixed in. The solution remained homogeneous with no separation at all.

Test 3: A third heaping tablespoon of NaOH was mixed into solution. Full separation occurred.

Results: 475ml of water & 125ml of alcohol appear to be fully separated. At most, a 10% loss.

Note: The measurement is very imprecise due to the fact the measurements are being taken off of a mason jar which only has marks every 100ml.

Conclusion: Isopropyl Alcohol separates with a 90%+ efficiency when mixed in a solution containing around 40 grams NaOH per 460ml of water.

Hopefully this sheds some light!
 
nah dont worry perplexed, high pH like 14, does not hurt spice, even after prolonged time :)

cosmic lion, your experiment is definitely interesting, thanks for telling us about it :).. but remember that even 10% of loss of the IPA can totally screw your yields, as alkaloids are VERY soluble in alcohols so even a little bit will probably be holding loads of your alkaloids..

proceed as your intuition tells you, and tell us the results, every information is very appreciated.. Personally, SWIM wouldnt go this way, he will go as he mentioned, as it seems less room for problems.. but keep telling us about what you do :)
 
SWIM reported that an evaporation of the alcohol in the experiment yielded a very fine layer of NaOH crystals. This could have been from rushed lab techniques during the turkey-baster suction of the alcohol off the water.

At this point, because of the excess limonene residue from evaporating a liter, it seems like the only solution would be a complete re-dissolve back into 200ml limonene. The limonene could be mixed with vinegar then the vinegar could be separated & evaporated, yielding acetate salts.

From there the paste technique could be applied.

SWIM will try some solubility tests to determine how much, if any, sodium carbonate dissolves in a 99% Isopropyl solution.

For the current situation SWIM will experiment by keeping a fan on the d-limonene, move to a desiccant chamber and hope for the best.

Once the final result is established, if the result is inaqequet, the vinegar & paste technique will be applied.

Thanks for all the help endlessness!
 
no prob, im just thinking here with you... SWIY is the one to be thanked for, for the experiments :)

maybe its simply that the NaOH is soluble in IPA ? I guess thats an even easier test to make..

btw, you think redissolving in limonene will be the only way? What about mixing whatever is evaporated with vinegar straight away, would it be a problem (maybe its already too much of a goo and the actual practical part of mixing with vinegar would be a problem?)

otherwise yeah thats probably what SWIM would do also, redissolve and so on..

but also do tell us if dessicant chamber/fan works

All these tests SWIY is doing will be of great use to SWIM once he makes his first limo extraction soon :)
 
The d-limonene is high-quality food-grade from Florida Chemical Company (a wholesaler, SWIM bought locally from a retailer)

It should be 97%+ pure

SWIM has, in the past, fully evaporated about 100ml of the d-limonene. There was a greasy residue which did not go away in any reasonable amount of time. After sitting out in open air for a couple weeks the residue went from greasy to very sticky.

I was thinking, if over 1 liter of limonene is evaporated it is bound to leave tremendous residue.

If SWIM takes the final evaporation product contaminated with limonene residue and mixes it with vinegar SWIM thinks that the residue will be near impossible to separate from the vinegar solution. 1-2ml of limo-grease in a 200ml solution of vinegar. One would imagine that this will just leave a disturbing greasy gloss on the top of the vinegar. Once the vinegar is evaporated the residue will be re-integrated into the result.

To avoid this, SWIM thinks the freebase\grease goo should mixed into 200ml limonene to dissolve the residue back into the limonene.

400ml of Vinegar can be added and separated. Assuming the vinegar is separated cleanly, the original limonene residue remains dissolved in the limonene.

The limonene would now be discarded, as it now contains excess limonene residue.

The vinegar can be evaporated to yield acetate salts, residue free.

The salts can now be mixed into a basic solution and pulled using a fresh 150ml of d-limonene.

The d-limonene can now be evaporated to yield a product that has only 150ml worth of limonene residue, instead of 1+ liter of limonene residue.

This approach seems to be worth a shot. It will be cool to see how the fan + desiccant chamber work out, hopefully the end result will be usable. If not, SWIM plans on trying this new technique.
 
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