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Crystalization failure. Options
 
5HT-2A
#1 Posted : 10/2/2013 11:47:36 PM

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Hey there, SWIM has been attempting heptane freeze precipitation with no luck, all SWIM has percipitated was white powder. I've done great things with naptha in both evaporation and freeze precipitation but have had no luck. Is there something I could be messing up to cause that? I've attached my evaporation results but I can't get anything like what people get with heptane.

link to album below.


album

 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
Nunyabiz
#2 Posted : 10/4/2013 3:57:45 AM

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Looks pretty good to me. The crystals in my avatar are from heptane re-x.
Nunyabiz attached the following image(s):
9484.jpg (33kb) downloaded 47 time(s).
 
5HT-2A
#3 Posted : 10/5/2013 1:20:05 AM

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Nunyabiz wrote:
Looks pretty good to me. The crystals in my avatar are from heptane re-x.


See those are the sort of beauty that I am aiming for! Have you ever had the issue of powder forming instead of crystals? and if so how did you deal with it? My usual method has been heating the heptane to boil then introducing the spice and after dissolving as much as possible pulling the top layer and slowly bringing to below zero temperatures. Is there a flaw I have been missing? I just wish I could get results like that!
 
alert
#4 Posted : 10/5/2013 4:06:28 AM
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When I recrystallize I just set the solvent at room temperature and cover it up with cheesecloth and let it sit like that for about a week or however long it takes for the solvent to evaporate. I am left with large crystal structures (with mimosa anyway). No need for a fridge or freezer that way.

Another thing people do is switch up the crystallization container from the fridge, to the freezer, to the fridge, to the freezer etc. This lets the crystals melt and then rebuild themselves.

Use a the smallest amount of solvent you need to dissolve the DMT before precipitating. Also, if you have a crystal already you can throw that in the solvent (when it cools a bit) to start crystallization on.

That first crystal you posted is nice though, nothing wrong with that baby! I'd say you are having decent results already Thumbs up
 
 
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