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Excessive naphtha after FP? Options
 
AstroChef13
#1 Posted : 10/18/2018 1:05:02 AM
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long story short, did my 4th pull following gordo tek. Definitely didn't let enough solvent evap before going to FP. I can currently see a decent amount of crystals in the dish but the extra solvent is pretty saturated with tiny crystals. Whats going to be my best course of action here? The dish is a glass dish with a sealable top. can I just flip the dish over and see if the crystals in the solvent will stick to the lid of the dish, or should I just pour off the solvent, heat it back up re evap and do another FP?
Thanks in advanced!!
 

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downwardsfromzero
#2 Posted : 10/18/2018 4:18:50 AM

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There's always Ostwald ripening, to increase the size of the crystals, or a mini A/B to reduce the volume of solvent going into the FP without having to evaporate naphtha.




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
AstroChef13
#3 Posted : 10/18/2018 7:27:56 PM
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downwardsfromzero wrote:
There's always Ostwald ripening, to increase the size of the crystals, or a mini A/B to reduce the volume of solvent going into the FP without having to evaporate naphtha.


I dont think Im fully grasping the Ostwald ripening... I ended up just pouring off the naphtha, letting the dish with already formed crystals dry at room temp with a fan then reheated the extra solvent it to get the crystals to melt back into solvent. Poured the warm solvent back into the dish with the already formed crystals and have just been letting it sit at room temp for almost 24 hours now. All the solvent is pretty much gone and theres pretty big crystal on one half of the dish that are pretty white. The other half has some smaller crystals and some goo. if this happens again how would one go about doing a mini A/B with the extra solvent?
 
downwardsfromzero
#4 Posted : 10/18/2018 9:49:15 PM

Boundary condition

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Mini A/B is described via the wiki already.

But I'm in a benevolent phase, so here is a summary:

Shake naphtha with a little vinegar.
Collect vinegar, add base to it.
Extract several times with small portions of naphtha that together add up to a smaller amount than the original volume of naphtha.
Repeat freeze precip on this smaller volume.

Ostwald ripening is in this case merely cycling between higher and lower temperatures in order to facilitate the growth of larger crystals at the expense of smaller ones. Swap between fridge and freezer every couple of hours, finishing in the freezer, of course!




β€œThere is a way of manipulating matter and energy so as to produce what modern scientists call 'a field of force'. The field acts on the observer and puts him in a privileged position vis-à-vis the universe. From this position he has access to the realities which are ordinarily hidden from us by time and space, matter and energy. This is what we call the Great Work."
― Jacques Bergier, quoting Fulcanelli
 
 
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