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Recovering d-Limonene trapped in bark/lime paste Options
 
Homo Trypens
#1 Posted : 2/13/2020 1:20:23 AM

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Edit and TL;DR:
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If an emulsion just won't settle at all, you can collect the emulsion layer and squeeze the NPS out through some filter (I used a wrap of about 5 coffee filters - tyvek should be better). This works really well.

The spice in this limonene turned out to most probably be oxide. So, note to myself, don't let moist bark mixtures dry out and sit for months, and if you do, don't bother trying to rescue your 4th pull Razz


Backstory:


In december, i did a Limtek extration. I mixed 300g mhrb powder with 400g CaOH, added just enough water to make a dough, then did three pulls with d-Limonene (after 1h, 1 day, 1 week). I salted out with FASW to get fumarate and converted that to freebase using sodium carbonate. I had slightly above 1% yield, and the bark wasn't fully depleted yet, i intended to do a fourth pull.

However, i didn't perform that fourth pull until last week. By this time, the dough had completely dried out. So i added water and rehydrated the brick, cutting softened pieces off with a knife until the brick was dough again, albeit with crumble. I let it sit for a few hours, stirred several times.

Then i added 400ml of d-Limonene and stirred again. When i tried to pour off the limo, almost none came out, maybe 10ml. I let it sit longer, but the situation didn't improve. I ignored it in the first three pulls, but there had been a bit of limo disappearing in every pull. Just now it was basically all of it.


Rescue (in progress):


I decided to boil the dough with a lot of water in a big pot. I pretty much hoped for a layer of limo to appear on top. I was prepared to distribute the ~8l of milky liquid to 3 smaller, more narrow glass containers for easier collection in batches. I didn't expect how it actually played out.

A layer did form on the top of each container. But it wasn't clear or yellow, it had the look of Baileys. It wasn't liquid either, it was kind of an oily thick creamy foam. I collected the foam from all containers into a wide mouthed glass bottle, diluted 1:4 with water and let it settle. I did that a few times. The water layer became less milky each time, less and eventually no sludge sank to the bottom, but the top layer kept consisting of that beige opaque foam. I left the bottom layers in the 3 containers. because i wasn't sure if the limo was in the top layer or still trapped in the sludge.

I poured the foam into a coffee filter and let it sit over night. In the morning, nice clear yellow liquid had come through, and i thought it was limonene. In the 3 glass containers, new foam had appeared on top! I collected that, put it into a new coffee filter dripping into the same glass as before. The used filter didn't contain sludge, it still contained foam, about half the original volume, it had gotten a bit darker and much oilier. I saved that.

After some dripping from the new filter, i noticed that the filtered liquid started having two phases, and side-by-side, it became clear that the upper thin one is limo, the rest was all water. When dripping stopped, this foam had also lost about 50% of volume.

I combined all the remaining foam, wrapped it in a few layers of coffee filters, and squeezed it as hard as i could, and substantial amounts of limonene came out. After done pressing, there was only little dark brown sludge remaining in the filters, clearly mimosa, probably with some CaOH. The clean limo layer now is about 60ml, and new stuff is emerging on top of the liquid containers as i type.

It seems the limonene is trapped in the sludge that sank to the bottom of my containers. I think it sank because it sticks with the lime also. I have now switched to stirring it all up, letting it sit for ~2h, then gathering the thin layer. The limo has that gasoline-style shimmer when it gathers on top, and it forms kind of a skin. I collect that skin with a spoon, which makes it become that foam.

Getting this far with the rescue took almost a week now Razz
Now with better understanding and adjusted technique, i'm confident that in another week, i'll have most of the lost limo back. From the looks of it, along with a bunch of spice!

I didn't take pictures of the dry mimosa/lime brick, the boiling pot or the first wave of foam. I'll take pics of the new foam, the filter residue and the recovered limonene soon.
Homo Trypens attached the following image(s):
foamtop.jpg (579kb) downloaded 43 time(s).
foamside.jpg (253kb) downloaded 44 time(s).
limoshimmer.jpg (400kb) downloaded 44 time(s).
collect.jpg (430kb) downloaded 44 time(s).
foamfilter.jpg (356kb) downloaded 43 time(s).
thinlayer.jpg (384kb) downloaded 44 time(s).
filterresidue.jpg (3,427kb) downloaded 43 time(s).
sepfunnel.jpg (566kb) downloaded 42 time(s).
 

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