My Friend followed the basic limetek allowing ample time between each step.
Under a gram was yielded:

500 Grams of powdered bark were used.

Approx half vinegar half water was brought to a quick boil and poured on.
The next day approximately 360 grams of Pickling lime was stirred in, in a gallon glass jar.



OK well it got wet on the more thick pea soap consistency, but not runny.

Another day went bye.
Entire mass is grey except a brown top that turns grey when stirred back underneath.
Entire mass smells like the typical basifying reaction.

Limonene was added, a total of three times over three days.

800ml Limonene was recovered.

5G Fumaric Acid was added to 100ml 99% IPA.
Plenty left on bottom so filtered through coffee filter into glass jar, along with an eye dropper on the side.

Ready for cloud formation.
Initial excitement; still intrigued, but only at absolute most appears to be under a gram of fumarate crystals sticking to jar and some other floaties.

3 days gone bye, a thin cloud still remains in the lower section but most of what is there has crashed.

Conclusion: 2-3 year old bark already powdered kept in freezer in original packaging allowed for oxidation?

Can this FASI-ed Limonene be FASW-ed to retrieve oxides?

Any other ideas as to what went wrong.

May the wetter nature of the lime-mush prevent limonene working.

P.S. A total of 75-80 ml FASI was added.

No more clouds form at this point. Just a clear squiggly integration when eye dropping in FASI.

Thanks for any help here.

Hope that wasn't too long winded for this section of the forum.

I have lots of experience with fasi and fasw, even a few fasa extractions under my belt. What i can tell you from experience is that it usually takes 5x or more day long or longer pulls to get a nice yield from a drytek using lime. The d-limo just has trouble getting to the FB molecules when its in the lumpy and viscous base-paste. Its best to do long pulls turning the jar often, and adding more water towards the end if you want to make it less viscous. Also, oxides i have found stay in solution and do not crash out with fasi or fasa. You can retrieve them with a bit of fasw, but it may also pull excess fumaric acid, waxes/oils, etc. Basically everything that's left behind using fasi/fasa instead of fasw. If you have annhydrous ipa/acetone its good to do a wash of whatever evaps from your fasw to remove any fats/oils or excess fumaric acid. fats oils can come from the ipa/acetone pulled into the fasw from the dlimo, and thats also where you can get excess fumaric acid. Which usually stays in solution with the dlimo/acetone or ipa as your crystals precipitate.

Most likely though, you just need to do more pulls from your plant material. If you want to get all/most of your alkaloids at one time you can go with a drytek, but do an acid boil first, reduce to a resin or small volume of thick syrup, then basify with lime or sod carbonate, and after a day dry with mgs04 (baked epsom salts). You can either use dry ipa/acetone/or d-limo to pull from your DRY based powder. You get most all alkaloids in one pull if you have enough solvent and is harder at first but much easier in the long run due to less pulls and less salting. Also, if you use acetone or ipa, you will just be making a more concentrated FB product upon evaporation that may/maynot be smokable/vapable as-is. There are numerous ways to cleanup if not. You could even pull from the acetone/ipa fb resin with d-limo and then salt to fumarates. I find it extremely enjoyable all teh different variations of dryteks you can do. Its best though to start small and work up to big extractions to work out the kinks beforehand.

Another cool thing about making a resin from your initial boil is that if you can powder it, its super easy to defat, just pull with d-limo, wet, fb, wait to react, dry with mgso4, pull again with d-limo or acetone/ipa. I find fasw pulls waxes oils on later pulls if no defat is done. Very cool.