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Negative limonene experience Options
 
5-htp
#1 Posted : 11/30/2012 3:11:23 PM
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 Smile

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).
 
dtrypt
#2 Posted : 11/30/2012 3:45:49 PM
if this was Reddit, I'd probably get downvoted for this... but
all I can say is STB man. I almost without fail get 1.4% off-white
and extremely smokable spice from STB.

I've done xylene and limonene with FASA and I just don't see the point
when you can simply basify and pull.

I understand if people approach extraction like a hobby and have time
to burn, but I just want the spiceCool
 
5-htp
#3 Posted : 11/30/2012 3:59:53 PM
dtrypt wrote:
if this was Reddit, I'd probably get downvoted for this... but
all I can say is STB man. I almost without fail get 1.4% off-white
and extremely smokable spice from STB.


you get downvoted for this ? Jup, I did STB's all the time with the previous bark and it worked like a charme. But I did other chemical stuff as well and the smells were kind of risky and of course unhealthy and so I wanted to go "clean" on this one. This is the reason I tried limo and the smell is really nice, compared to petrols..

maybe the limo wasn't clean enough (could just get orange oil no pure d-limo) or I didn't saturate the pulls enough. But now with most of the (salted) limo gone, I just don't want to waste anymore of the 500 G's of bark. I switched the supplier because I didn't want to import anymore so maybe it's the bark. No way to know with this technique.

When I'm done with this, I will do a 100G STB like I used to and will know for sure.

Seems like one is either lucky or needs some experience with limo, FASI/FASW. So doing 500 G the first time wouldn't be clever. I was just so sure after reading everything that I could manage this and would just have to do one big extraction which would last me for months..
 
obliguhl
Senior Member
#4 Posted : 11/30/2012 4:56:20 PM
I agree that BLAB can be a bit tricky, especially because there are so many steps and at which you can fail (lose spice). Its a great tek if you want a)full spectrum spice (but then i would have kept the oils) b)something for ayahuasca or pharma preperations.

And reddit users downvote everything, it does not matter if your comment is intelligent or not. If it goes against the "hive mind" (= the reddit culture) it will be downvoted.
 
5-htp
#5 Posted : 11/30/2012 5:03:07 PM
obliguhl wrote:
...Its a great tek if you want a)full spectrum spice (but then i would have kept the oils) b)something for ayahuasca or pharma preperations.


You think the oil, I separated by melting the furmarates and which didn't smell or taste other then some vegie oil, contained some of the full spectrum alkaloids ?

Still don't get the reddit thing Razz
 
5-htp
#6 Posted : 11/30/2012 5:46:40 PM
One other thing I notice with this limonene method compared to stb is that you put your self at more risk because there is much more time needed to work it all up. I personally am not the kind who hides after blinds as soon as it gets dark (here it's winter now Smile), so if doing this for the whole extraction/workup procedures it would be even more suspicious (I live in a suterrain place with windows to the ground).

I try to work everything in my normal schedule as to raise no suspicion (living in a small town gets people really bored, so they wanna know what everybody is up to).

 
 
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