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BLAB: Emulsion layer during precip phase?!

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obliguhl

obliguhl

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So, 500g of bark from jimjamshop was extracted using a slightly modified BLAB technique. The container was 5l big so it had to be used more water and lye. Also, 200ml pulls were necessary because it was next to impossible to get any orange oil back because you can't squeeze the container to get lyetea free limonene.

4x200ml pulls were performed and FASI added. Precip started and now after a week or so there'S a thick snowish layer that won't go away.

Yield is a measly 3g and it looks like it'll be it because not much is percipating now.

What went wrong? After hearing about fantastic yields of 1.2-2% I'm dissapointed. Maybe the orange oil wasn't saturated enough due to the bigger pull size?
 
Well, it did not fall to the ground like the rest of the fumerates, it was somehow trapped in the d-limo. Maybe because of the orange peel residues? Had to filter it. It's now dissolved in 100ml of water, waiting for the excess fumeric acid to drop out...
 
interesting! So did you see it suspended in the limo, was it very obvious, or what gave you the idea of filtering? and how long did you wait for precipitation?

btw, AFAIK there shouldnt be any excess fumaric acid.. I think people already tested that fumaric acid doesnt precipitate when adding FASI to pure limo, so it should only be pure fumarates precipitating from the alkaloid-full limo (correct me if im wrong.. )
 
Yes, after a week of waiting, the clouded layer did not seperate, so i put both layers in different containers and filtered the clouded one. Good to hear about the exess fumaric acid..so it can go to evap stage...thanks
 
I always wash it once or twice with acetone to get rid of the d-limo. I know d-limo is non toxic and acetone isn't, but you can't gat accurate weights if the fumarate is all sticky with d-limo. The acetone evaporates so quickly and completely, it seems worth it.

Pokey
 
Seems worth it if you'Re in a hurry, otherwise a water evap cleansing will do fine i guess.
The wet/uncleaned yield is now up to 10.3 as another 2.2g could be salvaged and there's more percipating out. Really wonder about the final dry yield.
 
So i poured some acetone over 2.5g of material and collected the undissolved bits...went down to 1.5g...so the loss is actually 60%...ouch! So a final yield of 4-5g fumerates is more likely....:surprised
 
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