*the poster is interpreting all of these communications via methods of divination and thus any reference to "self" or "I" should be understood to be translated from Galactic Hyperspeech into basic English and not in any way reflect upon the actual physical poster*

Followed all instructions to a T, have successfully utilized this method before.

Pull 1) resulted in some fairly nice crystals after a night in the freezer

Pull 2) has not precipitated whatsoever.

the only reason one could see for this is that between pulls additional base was added to help dry the mixture after it had absorbed a bunch of solvent from Pull 1. So this got me thinking, is there a prefered amount of time to wait between pulls or after basing? Were the goodies somehow left behind as a fresh round of basification took place?

also how could one hypothetically seperate water from a product laden naptha batch should water have been accidentally spilled into the dish during the heat bath

Try pulling again but reusing your solvent from pull 1 - that's assuming you did 2 separate pulls. What base did you use?

To separate the water, if possible carefully pour off most of the naphtha and then... well, the choice is yours. You could soak up a few drops of water with a pinch or two of salt or bicarb, or if you have a long, thin glass (Pasteur) pipette you should be able to remove the water with that. If you've managed to pour off virtually all of the naphtha you could pipette the remainder away from the water or even stick the container in the freezer and subsequently pour off the remaining naphtha. If you have more than a few drops of water then ideally you'd use a separating funnel.

If you don't have any pipettes or a separating funnel and the water is essentially clean you could freeze the whole lot and then pour off the naphtha. Then you'll just have to work out what to do with the crystallised product sat on top of the block of ice.

Frankly, I'm making this up as I go along but hopefully it provides you with some FOOD FOR THOUGHT!

yes it did!

and I used the exact brand of lime specified in the tek. maybe I didn't let it heat up long enough? not sure but pull 1 went great and resources are plentiful so I'll just have to chalk my mistakes up to data costs and being a noob.

These things can take some time to 'digest', you may find more goods show up next week (you haven't got rid of any of it yet, have you?) Either that or your first pull is super efficient?

One other possibility I can think of is that small amounts of aromatics in your naphtha are inhibiting freeze precipitation. You could try back-salting into vinegar or citric acid solution then adding base to that and re-extracting into a much smaller volume of naphtha.

yeah I did. I tried to just gently pour the liquid off into the precip. con. but the water made it so sloppy that at just a slight tilt (done carefully) all sorts of barkmush came out with it. With no other suitable containers I just dumped and rinsed and re-limed the mush to help it dry out for a few moons.

although slightly on topic of a different thread around here, the original naptha batch that wouldn't precip. in the freezer was poured back into the mush and let sit while covered overnight, then was put back into a precip. con. and then the fridge, then the freezer, and pretty spectacular results were had.overnight with this.room temp technique. no heat bath whatsoever.

the batch that was disposed of was done after the room temp naptha was reused

You *really* do need a glass baster, some small pipettes or a decanter in order to avoid a great big mess.

If you're careful when extracting, you won't have solvent retention in your bark mush... Essentially, the solvent becomes trapped in "pockets" of aqueous mush, and those pockets become smaller and smaller as they are broken apart with stirring/handling. Eventually, a nasty emulsion forms... Instead of stirring the mush, place it in a large shallow pan (pyrex casserole or baking dishes work well), then tilt the pan back and forth to move the solvent over the mash; Don't stir the mash with solvent in the dish! Dump the solvent out of the dish, stir, then re-add solvent.

If you must stir with solvent in the dish, use a glass stirring rod or the handle of a stirring spoon. Don't use a spoon, that's the worst for trapping solvent.

You shouldn't need to add much base to the mix after each pull.. Also, make sure to add back a little water; Dry lime soaks up naptha just as well as it soaks up water.

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Water can most easily be removed with a small pipette. You can get these on Amazon for cheap.

I always thought stirring the mush gently was necessary for it to saturate as much of the bark as possible?

otherwise aren't you just interacting with the mush on top?

I usually dont need to relime so much this time it just turned into a slush and cluster****