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Heptane Recrystallization Imperfections..Pictoral

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H

HotTuna

Rising Star
Hey everyone...This is my first post as full fledged Nexian. Pretty excited...

Anyway, SWIM did a heptane re-x and found this image online which accurately describes the issues at hand.

About 1g of spice was Re-X'd with 30ml warm heptane. Mildly agitated until the initial spice was dissolved..clearly some oils were dissolved, but MOST stayed undissolved and was removed from the solution.

Solution was slowly cooled in a water bath and even more goop fell out of solution leaving clear heptane...xtals formed on top of the goo. boo. But nice xtals, nonetheless.

Swim feels like they are losing a lot of yield to get white xtals, and that there's left over spice in the yellow goop.

Is swim doing something wrong? What about technique, re-x containers? temperatures? anything? need multiple re-x?


SVzBD.jpg
 
1) Freeze heptane to get out remaining spice.
2) do more heptane pulls on the goop
3) STB's pull more oils and unwanteds than A/B thus more is lost in the purification process
4) it may take multiple recrystalizations to get a pure white product...with additional yield loss..this is quite normal.
 
Thanks! SWIM siphoned off clear heptane and it was FP's and there are white small crystals formed as to be expected from a FP..... good news.

Anyway, is the current process is ok? parameters/temperature are good? Should swim try to separate the white Xtals from the gunk or just re-dissolve it all in fresh solvent and pull the goop off the bottom again before anything crystallizes?

If SWIM trys to do some pulls from the pure gunk, should the approach be the same as above, or should swim fully dissolve it all and do slow cooling?..SWIM found about 140°F will suffice to get it all the oils dissolved..
 
HotTuna said:
Thanks! SWIM siphoned off clear heptane and it was FP's and there are white small crystals formed as to be expected from a FP..... good news.

Anyway, is the current process is ok? parameters/temperature are good? Should swim try to separate the white Xtals from the gunk or just re-dissolve it all in fresh solvent and pull the goop off the bottom again before anything crystallizes?

If SWIM trys to do some pulls from the pure gunk, should the approach be the same as above, or should swim fully dissolve it all and do slow cooling?..SWIM found about 140°F will suffice to get it all the oils dissolved..
Click to expand...

I'd recrystalize your white xtals with yellow in them again and do a seperate rextalization on the yellow goop.

I personally don't want my heptane to be hot enough to dissolve the oils. I get clear or white xtals when my heptane is clear.
 
Understand too that the yellow goop you are left with at the end of the day will likely be plenty active. It's just nice to separate as much as possible what you know is ultra pure.
 
Uncle Knucles said:
Understand too that the yellow goop you are left with at the end of the day will likely be plenty active. It's just nice to separate as much as possible what you know is ultra pure.
Click to expand...

Agreed, save the yellow goo!!
 
Both of you, thanks.

Swim will continue the same process, but less heptane @ same temp. Appx 120°F and siphon the settled goo....

what does one do with the goop once all spice has been pulled from it?...SWIM's good is in the freezer...solid.
 
SWIY used too much heptane and/or too hot of a temperature, which allowed the goo to dissolve, along with the dmt (the color is an easy indicator, as it should remain clear and separate from the yellow goo, and not have that yellow tinge) SWIM had this issue once (too hot) and all swim had to do was wait for it to cool down enough for the good to precipitate, then suck it out with a dropper and watch the pure shards grow!
goodluck!

(and yes, save all the goo! SWIM loves the goo almost as much as the pure stuff!)
 
I am a big fan of A/B with slight acidification in vinegar (pH=4) and multiple (3) simmers, filtration, reduction and decanting, and then basification to pH about 12, and 5 pulls with hexane. White spice falls out every time, no gunk, no nonsense, no re-crystalizations. Just one freeze precipitation and the product is damn clean and purty damn powerful! Nice mild smoke and instant launch.
 
Rivea said:
I am a big fan of A/B with slight acidification in vinegar (pH=4) and multiple (3) simmers, filtration, reduction and decanting, and then basification to pH about 12, and 5 pulls with hexane. White spice falls out every time, no gunk, no nonsense, no re-crystalizations. Just one freeze precipitation and the product is damn clean and purty damn powerful! Nice mild smoke and instant launch.
Click to expand...

SWIM wants to try an A/B extraction for that reason. I've read them all, but which one do you prefer?


...SWIM just RE-X'd again. Appx 650mg in 12ml heptane. Dropped the heptane temp to about 100-105F, seems to be better at the not letting the goop dissolve, but harder to get the xtals to dissolve, but there was some xtals locked in the goop, so the goop was agitated and expose the xtals to solvent. The agitation caused some goop to go into solution, but it seemed to drop out of solution relatively quickly and settle back to the bottom....It's a finicky process.

Results coming
 
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