Hello everybody. I have a string of questions please, if you dont mind. I will do my best to be succinct

I recently took up the hobby and felt freebase was the right path. Included pics are my first extraction. Q21Q21 lime tek with wundbenzin 40/60 (hexane/heptane from what I think I have learned), absolutely performed to the letter of the tek, inputs weighed. That was 0.51% recovery on the first pull. I have yet to take the process further but will adhere to the schedule outlined in the tek

The only deviation was that the bark/vinegar/water/lime mix was extremely dry before adding nps, with no visible moisture on the bottom of the glass. About the consistency and appearance of good compost/earthworm castings but dry and crumbly like cheesecake base before you press it into the cake tin. Best analogy I could think of, sorry

No aqueous phase was observed after the addition of nps either, but I proceeded. Some solvent loss was noted, perhaps 25% total. There were also some very tiny crumbs of bark that rode on the solvent through the sieve into the precip dish, maybe half a dozen which I picked out with a scalpel, but some tiny flecks were unrecoverable. Things appear to have gone smoothly anyway after freeze precip and product has all the physical characteristics expected, melts beautifully with a golden hue to the resulting oil and leaves no chalky residues, smelling of sickly sweet faint plastic. So I feel like if there is calcium contamination (I am not even sure if that is possible tbh) that would present as chalky residue left behind on vapourisation?

So the other questions are about the mixing of teks and specifically the addition of a salty brine step such as in the max ion tek, but applied to the Q21Q21 lime tek at perhaps the third or maybe final pull so as to force those remaining alkaloids into the nps more drastically. As I would be adding moisture volume, this would also kinda 're-wet' my material and allow a distinct polar/non polar layer to properly evolve during the extraction. That is my thought process. Please poke holes at will

Can this work, or do the salt and calcium present a problem and react together to form unwanted compounds? I assume the only thing detrimental that could be formed here would be calcium chloride but I have no background in chemistry and am not even sure if that is possible in the first place, much less whether or not that would be carried over into the final product? Can somebody help please? If you rather give me links so I can teach myself instead of just giving me the answer then I would also be most grateful for that

It's a lot for a new fella to take in all this stuff and it may very well be that I proceed to the letter on this extraction anyway, just to be faithful to the tek, but I would love to know more about this for the next round, where I might like to try a more wet version of the same tek. Other teks will also be performed in due course for comparison

Thanks for your help and have a nice day

https://tinypic.host/image/1705740574066.Fxf41
https://tinypic.host/image/1705740574059.FxPS6
https://tinypic.host/ima...01/20/1705740574076.jpeg

Pictures look great, I would continue doing the rest of the pools with the same tech and you should end up with a good yield.

Thanks for your thoughts Kmk, I proceeded with the second pull as normal and it is still in freeze precip stage but already shows good promise, maintaining bright white colour so far

In the meantime I did some research to attempt to answer my basic questions and found that indeed when salt and calcium hydroxide are added together, the do a 'double displacement reaction' and form some amount of sodium hydroxide and calcium chloride. I assume the added base is not an issue but perhaps the calcium chloride might be...

However after examining the specifics of that, I find that calcium chloride is highly polar and insoluble in heptane/hexane. So I feel like this max ion salt step may be possible without breaking anything, I dunno if it is as simple as that to figure out or if there are other side reactions potentially occurring that I have not considered. I don't know anything yet and am only emulating like a monkey at this stage

And I guess I also answered my own question about calcium contamination in the first pull at the same time. Will continue to update with other questions and the results of my efforts

Cheers

That's not the whole picture and somewhat wide of the mark tbh.

The salt adds sodium and chloride ions to the system and these remain in solution until the solubility product of any given combination of ions is reached. Since calcium hydroxide has by far the lowest solubility product in the lime/salt/water system, the amount of undissolved lime remains largely unchanged. The double displacement would occur in the opposite direction and would only be observable upon mixing of sodium hydroxide solution with calcium chloride solution. In all but the weakest solutions calcium hydroxide would precipitate out until the solubility product of calcium and hydroxide in the remaining solution drops to the maximum value for calcium hydroxide. One upshot of this is that a higher amount of hydroxide will still force the precipitation of calcium hydroxide even if the amount of calcium present would be less than the nominal maximum for calcium hydroxide alone.

Furthermore, both sodium hydroxide and calcium chloride are so highly soluble that mixing concentrated solutions of the two would cause the precipitation of both sodium chloride and calcium hydroxide. This should be sufficient illustration such that one can infer that adding sodium chloride to lime paste will not cause any addational calcium to go into solution since it is always the least soluble components that will precipitate - i.e. in this case, NaCl and, overwhelmingly, Ca(OH)₂.

https://en.wikipedia.org...i/Solubility_equilibrium
https://de.wikipedia.org...6slichkeitsgleichgewicht

Calcium contamination is more likely if lime particulates get carried over in NPS pulls that are then washed with vinegar for alkaloid recovery, e.g. with limonene. You've used naphtha which, besides allowing for freeze precipitation, also seems to be less inclined to picking up lime particles, perhaps because of both density and viscosity being lower than with limonene.

Thanks DFZ for helping me understand

I am trying pretty hard to understand things properly rather than just copying, but it is kinda over my head at the minute. It's going to take a while I guess before I understand the chemistry properly

in the meantime, we continue slowly on following the teks and noting observations

second pull
https://tinypic.host/image/1705902328975.coWek