Perfect naphtha separation?

[strtman]

I would like to submit a method.

When the naphtha has floated on top of the basic sludge one has to separate this. In order not to take out some droplets of basic sludge, I don’t do this to the end. A very thin layer of naphtha remains in the vessel.

The separated naphtha is put in a thin glass container. It stays there for about twenty minutes. Again the naphtha is separated (leaving the last bit in the thin glass container) and put in a jar for freeze participation.

After the freeze participation the crystals are taken out to dry.

With this method I have deliberately sacrificed some naphtha. But the naphtha that made it to the freezer is ok.

Why this method? Because I did my first re crystallization and I am shocked how much yield is lost. About half of it. I think that with my suggested method I certainly loose some DMT but perhaps not so much and it is an easier way to get it.

I have the unpleasant feeling that the re crystallization not only took away some goo but much of my DMT too.

What do you think?

 

[downwardsfromzero]

Yes, it's well worth being careful in the first place to have a purer initial extract. Your method as described is (or should be) pretty standard.

Transferring your naphtha from the base soup and into an intermediate jar before putting it into the freeze precipitation container also eliminates virtually all of the base soup contamination.

[Reading your recrystallisation thread, it sounds like you used too much naphtha. 5 - 6mL would have done the job. You want only as much near boiling naphtha as will dissolve your spice.] Edit: Actually this would only apply if you were going to freeze precip., and it seems you just evaporated. I'd suggest using less solvent and freeze precipitating.

As an example, I have known of 600mg spice being recrystallised from 6mL boiling naphtha and yielding 580mg pure white crystals from a freeze precip. The main contaminant was a tiny bit of basic sludge.

Your lost yield is still dissolved in the orange goo. It won't be all contaminants. If you still have the orange-coloured oil, it can be extracted some more as it still contains some goodies. If you separated it from any basic sludge, it could even be used as it is. Or you could consider a mini A/B for a cleanup: dissolve the goo in a little white vinegar, re-basify with, e.g., sodium carbonate and pull with acetone or naphtha.

It's possible your initial pulls were a little on the warm side as this may tend to pull more orange goo.

Good luck, stay safe!

dfz

 

[strtman]

Thank you for this information.