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purification teks compared

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DiMiTriX

DiMiTriX

Rising Star
ok swim has an idea to share.. alchol/water precipitation..swim has the issue of not pure solvent,so he was wondering to dissolve spice into alchol,and than put into it a conentrated solution of na2co3(carbonate) maybe at 1:6 ratio,the higher the better i think..and than wash the freebase precipitate with water. what do you think?
or would be better dissolve it into vinegar,than basify with na2co3 and filter the freebase precipitated?
 
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DiMiTriX said:
ok swim has an idea to share.. alchol/water precipitation..swim has the issue of not pure solvent,so he was wondering to dissolve spice into alchol,and than put into it a conentrated solution of na2co3(carbonate) maybe at 1:6 ratio,the higher the better i think..and than wash the freebase precipitate with water. what do you think?
or would be better dissolve it into vinegar,than basify with na2co3 and filter the freebase precipitated?
Click to expand...
What is SWIY really trying to achieve here? He tries to purify spice, yeah, but from what? This is what you ought to be asking before thinking of an approach.

btw, dissolving the spice in vinegar and then trying to precipitate it out with sodium carbonate is not going to work. Why, it is unclear, it just doesn't work. And adding alcohol in concentrated solution of sodium carbonate will cause precipitation of a fair amount of sodium carbonate and will also cause a partial separation of the water:alcohol to two phases.

So basically you have no goal (purify/clean spice form what?) plus what you propose seems problematic.
 
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swim used a stain remover to get the spice out..it's 70-80%,10-12% ciclopentane esane,7-10%dichloropropane,3-5% n-esane and 5% pentane
swim precipitaded it by cold and than give it a wash with carbonate solution, it's passed 2 hours an it still smells of it,is it normal? maybe i could try to do a paste with carbonate,let it dry,crush it and than wash with etanol? dunno purity of this solvent,but it could have some high boiling point sols into :? this could be just my paranoia :)

spice is off-white,pale pale yellow,nice crystals,they were tiny globes

i could buy citric acid and try salify citrate and than freebase it, but i have ascorbic acid,maybe i can do ascorbate and than preipitate it out? noone tried isn't?
 
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DiMiTriX said:
swim used a stain remover to get the spice out..it's 70-80%,10-12% ciclopentane esane,7-10%dichloropropane,3-5% n-esane and 5% pentane
swim precipitaded it by cold and than give it a wash with carbonate solution, it's passed 2 hours an it still smells of it,is it normal? maybe i could try to do a paste with carbonate,let it dry,crush it and than wash with etanol? dunno purity of this solvent,but it could have some high boiling point sols into :? this could be just my paranoia :)

spice is off-white,pale pale yellow,nice crystals,they were tiny globes
Click to expand...
If I get you right, SWIY used this stain remover to pull freebase spice from basic solution, then freeze precipitated it and then he washed the spice crystals with sodium carbonate?!?!?

If you want the smell of the solvent to go away (the way I read you it appears that SWIY's problem is that his spice smells like solvent) then just dissolve the spice crystals in ethanol and let evaporate, maybe do this 2-3 times to make sure all the non-polar solvent evaporates out of the crystals where it may be trapped.
 
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ok..so this would be the route for further extraction swim thinks..he could get heptane dichloropropane mix,the first bp.98 the second 96°c so he could boil some solven off crystallize by freezing and recryst with etanol and bingo..no danger of impurities swim thinks and hope
 
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