Looking for some confirmation...please?

[dooby]

Hello,

From these pages I gather that pre-evaporation of the nps can facilitate freeze precipitation of poorly saturated pulls.

I also read (and experienced) that super-saturated pulls will form crystals even in the refrigerator...

I do not own a freezer and pre-evaporation of my solvent is something is wish to avoid...

So I have been looking into the back-salting/freebase reconversion techniques but before actually attempting this I would like to have some confirmation that my train of thought is on the right track - or some education if it isn't

I will describe the steps I plan to take, please warn me if there is anything in there that could possibly contaminate or kill my yield

1 Carefully decant nps from fridge-precipitated crystals
2a Combine decanted volumes of nps
2b Retrieve fridge-precipitated crystals with warm naphtha for re-x
3 Add vinegar dropwise to the decanted nps, occasionally stirring or shaking the mixture
4 When naphtha is clear again, add some more vinegar and shake/stir one last time
5 Allow naphtha/vinegar to separate
6 Decant naphtha, let vinegar evaporate
7 Add sodium carbonate (equal amount of evaporated vinegar, or a bit more?)
8 Add water to moisten the aforementioned mixture, allow reaction to take place
9 Pull with warm (or hot) naphtha (adding dropwise)
(10 Pour naphtha through coffee filter?)

This should hopefully result in all the spice that wasn't fridge-precipitated to be sitting in approximately 100-125 ml. of naphtha rather than nearly 1000 ml.
This would then once again be fridge-precipitated, remaining naphtha will be evaporated...

I know there are other/better/less-toxic ways of going about this, but for now I'll have to make do with the materials/products I have (no freezer, no fumaric acid, no anhydrous acetone/IPA etc...) so please take this into account when formulating your answers

Much obliged!

PLUR

 

[Du57mi73]

It would help if you knew what your expected yeild was so you can accurately use enough solvent and vinegar. But I don't see anything wrong with your proces. What I might also suggest that since you don't have a freezer, and since temperatures are dropping outside(where I am) that you might achieve even colder temperatures by sitting your jar outside. Also, it looks like you are precipitating, reabsorbing it into new npps and then combining that with your original nps. That original fridge precip is not necesarry(unless that's something you've already done. Lol).

 

[dooby]

Thanks!

Yeah, I already fridge-precipped some crystals, these will be recovered for re-x, the decanted nps will be treated as mentioned above...

Next time I'll probably skip the initial fridge-precip and salt everything out in one go...

I started from 200 gr. of mhrb powder, so the yield could be anything between 1 and 4 gr....

I kept my basic solutions so if the yield is on the low side I can do additional pulls

I'll dry the already fridge-precipped crystals before re-x so I can guesstimate how much desirables could be left in the nps...

Thanks again...

 

[dooby]

Questions regarding steps 8 and 9...

1. How much would be needed (approximately) for the reaction to be completed?

2. Should I let the paste dry before pulling or should I add water before pulling making this a mini-STB?

3. Should I filter my pulls if done on the dry paste?

Thanks

PLUR