I want to share my experience working with limonene. After I read all I could find about limonene teks I started performing a BLAB extraction by the tek and aproached it with the FASI method. Well, this was nearly 3 weeks ago and I'm still trying to get the goods out of my huge 5 Liter HDPE tank.
Here is what I have done with 500G MHRB:
- soaked the bark in 1 Liter 5% vinegar for 3 days
- added 250 G Lye, dissolved in 500 ml water, shook hard
- filled the container with dest. H2O, leaving enough room for the pulls
- added around 200ml limonene for the first pull, mixed by moving the container around some time and have let it sit for 24 hours to get the limo clear. next pulls have sat a bit longer and volume of solv. was decreased
- collected about 600 ml limonene which I dried with anhydrous MGSO4
- filtered the limo because it won't clear on it self
- prepared FASI, added FASI (100ml at first, 100ml later as there was still clouding) really slow and precip occured (that was a beautiful thing to watch). Have let it sit for a day +1 (No Crystals appeared, more like wet salt collected at the bottom).
- Separated limo from the precip and filtered it
- Dried the furmarates in the oven at 100°C. Then ramped the heat up to 150°C and the residual oil came out of the molten furmarates. Moved the evap dish up at one side so the oil collects at the side. It had no smell and taste at all.
- Scraped together the brownish/black furmarates and washed 3 times with IPA. I got 4G ash-grey furmarates which looked quite okay.
- I did the SC-paste conversion (pulled with acetone 3 times) with half of it and got around 750mg brown oil that crystallized. That was nice but got me thinking about total yields being very, very low.
- tried washing the limonene with H2O for pulling again and it clouded really heavy. Then I read of someone, prefering one strong base wash. So I added lye and put the container in an water bath. It cleared up but after letting it sit some more, it ate through the container. Wuuuuuusch limonene is in da house. I didn't notice that the second container was not HDPE but PET. Bye, bye limonene.
- So I went for naphtha, washing the residual solvent in the main tank with small amounts, pulling and collecting for later workup. I did 3 pulls to get rid of the limonene (100ml total) and pulled 3 times with 50 - 100ml naphtha, keeping the whole thing warm in a huge bath and slowly moving the container around for some minutes until I could see the naphtha turn yellow and letting phases separate for some hours.
- Crystallizing didn't work, so I boiled it down last night in a double boil setup with a fan blowing on top. The whole place smelled like limonene and what a surprise, I ended up with 50ml limo (after 12 hours 50°C-fan-evap).
- Did a search on evaping limo and found the FASW approach. Did it with the 50ml limo and as I saw the emulsion which probably won't turn away in my life, I thought, how many fuckups can there be with this solvent ? I should have pulled with vinegar.. I hate the FASW-approach on limo. I hate limo

Well there have been some workups in between and I have around a Gramm and a half of JimJam FB and Furmarates precipitating in either limo from FASI and I have some FASA emulsion plus the huge soup-tank from which I will pull with more naphtha as soon as my supplier stocks up again.
It would have been so much nicer, if I had pulled with naphtha/toluol/hexane first and used some limo for the remainder. This is a nightmare (a very beautiful of course).