Q21Q21's dry tek: D-Limonene is not separating

[Jan e Kharabat]

Hi,
SWIM's doing the q21q21's lime tek. SWIM did 3 pulls with Washbenzin which went well, the solvent and the mixture remained separate. For the 4th and 5th pull SWIM added about 100ml Orangen-Terpene which pretty much dissolved into the mix and it became much soupier. There was a really thin layer of solvent on top which couldn't be separated without pulling in the gunk below.
After waiting around 2 hours SWIM tried to tilt the bowl and pull with a 2ml pipette from the edges where the separation line was barely visible. The solvent was pulled 1-2ml at a time... which was not an easy task! After that SWIM put the bowl on the radiator and waited another hour after which there was another equally thin layer which was separated the same way. In total SWIM was able to get around 60ml of brown and cloudy solvent. The rest did not separate and had to be evaporated from the mixture to regain the same consistency.
SWIM would like to ask what the likely cause could be and what could be done to avoid something like that in the future.

The following Orangenterpene was used

https://www.ebay.de/itm/Orangenterpene-D-Limone-100-1-Liter/132961041751?hash=item1ef5187d57:g:aYYAAOSw~2xcbkSf

 

[downwardsfromzero]

What colour is the terpene solvent when it comes fresh out of the bottle?

Orange terpenes might not necessarily be pure limonene and can present reactivity issues when used for extraction. One time I had this problem I ended up evaporating the whole thing down to a crusty powder over the course of a week and trying again with far less water.

Naphtha/Waschbenzin is fine with a more liquid consistency for the lime paste but with limonene it needs to be like dough (Knete).

 

[Jan e Kharabat]

It's colorless fresh out of the bottle. I tried 2 different consistencies but with same results, the solvent straight up dissolves into the mix. I've dried up the mix again, had to evap all that Limonen... Could it be that the lime is not enough? Could adding salt be helpful?

 

[downwardsfromzero]

At this point it'll be best if you can describe exactly what you've tried so far in as much detail as possible - particularly what the consistency was and how you mixed the solvent with it.

I'd make it really doughy and fold the limo through with a fork.

Some of the limo will always disappear into the dough at first but repeated pulls should make up for this loss.

 

[Jan e Kharabat]

Well I soaked 50g of bark in 100ml of 5% ascetic acid with a dash of citric acid. I then added another 100ml of Water followed by lime which I didn't exactly measure but I think it was most likely between 30-40g. I mixed until the it turned dark and evaporated some of the water to get a soft dough type consistency. I then did my 3 Washbenzin pulls which went without a problem. Then I did my first Orangenterpene pull which also went relatively ok. I used 100ml of Orangenterpene, some of it was soaked up by the bark mix but the layer which separated was still thick enough to be decanted. Afterwards however, the consistency had become more liquid. I then waited another day and put the bowl on the radiator to evap some of the fluid. The consistency was more liquid than the initial dough like consistency when I made the second pull. This time the limonene straight up vanished into the mixture and the consistency became more fluid, like a very thin soup. There still was a very very thin layer of limonene on top which couldn't be decanted so I removed it with a small pipette and then filtered it to remove the gunk. Afterwards I evaporated all fluid until the mix became a dry powder. Next I will try to add as little water as possible, keep the consistency dry/porridge like and add the limonene again. If it separates better, it would be because of the consistency, if not, then the Orangenterpene is more likely the problem.
Also, the 50ml limonene I pulled with the pipette the last time was really saturated... a whole lot of spice crashed out of it on adding FASI. So I assume the bark is exhausted or nearly exhausted by now.
Also, I had some yellow limonene left from the first limonene pull, I had already added FASI to it and collected the crystals. Just out of curiosity I added it to the limonene from the second pull. I think the left over FASI in it reacted with the limonene from second pull, the solvent became cloudy, but two layers were formed, a transparent one on top, and a cloudy one at the bottom (the bottom one is from the second pull). Initially some crystals crashed out and formed a layer between the two. I then added some more FASI which sunk into the bottom layer and resulted in more crystals crashing out which settled at the bottom. I am not sure what exactly is going on here... but it sure looks a bit funny. Do you have any idea what could've caused the separation of two layers? they are both the same solvent, it's just that one is spice saturated and the other has some left over FASI in it...