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Really silly mistake Options
 
ragabr
#1 Posted : 2/3/2010 6:28:39 PM

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So SWIM extracted from 100g HMRB, treating overnight with a warm acetic acid solution and then basifying the next day (hooray stoichiometry!). Pulling with heptane, everything was coming out beautifully, huge amount of crystals through freeze precipitation. She did a activated charcoal wash, and then a sodium carbonate wash.

After freeze precipitating again, and evaporating, SWIM was left with maybe 1/4th of the crystal mass she had before the washes. SWIM still has the excess solvent, and it's in the freezer. She thinks the crystals are gone though, and the reason is she used chilly water, from the fridge Brita, during the washes. SWIM saw the solvent go cloudy, as soon as it hit the water and knew she had a problem. In her frustration, she forged ahead, trying to warm the container with running hot water. SWIM thinks it was too late.

Please learn from her mistakes.
PK Dick is to LSD as HP Lovecraft is to Mushrooms
 

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endlessness
#2 Posted : 2/3/2010 6:38:45 PM

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cold water wouldnt be any problem in washing, because dmt is LESS soluble in cold water... did you throw anything away? dmt doesnt just dissapear, its there somewhere.. So whoever is reading this, if you ever come across some problem, dont throw things away it can 99% of the times be saved....

Was the water basified with sodium carbonate in all the washes?

How did you do the activated charcoal wash done?

how much solvent was used to dissolve the crystals for the wash?
 
ragabr
#3 Posted : 2/3/2010 7:23:45 PM

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The water used during the washes was thrown away, everything else has been kept. The water was basified only for the first wash, following that was a charcoal wash and a plain water wash.

For the activated charcoal wash, she just pinched some AC into the warm solvent, swirled and filtered through a coffee filter. The solvent used was ~25mLs, heated.

Thank you for the help!
PK Dick is to LSD as HP Lovecraft is to Mushrooms
 
mumbles
#4 Posted : 2/4/2010 2:17:58 AM

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etherealsamba wrote:
my guess would be that since you used pre chilled water, it might have messed up things.. reason being, the water is cooled directly with refrigerant, which is freon..

Smile might be a problem people should be aware of..
I don't think the two come in contact. And even if they did I don't think it would make any difference. The use of activated carbon will have stripped away some of the DMT, and a second recrystalisation will of course reduce the yeild. With a STB the lost yield is rubbish plant gunk and lye but with an a/b and freeze precip swiy already has very clean spice so the DMT loses are much larger. You are supposed to use sodium carbonate in cold water for the washes so relax. Now if your solvent was so super saturated that the spice precipitated out on cooling after contact with the cool water there should have been a visible layer. Also the water needs to be based for each wash, otherwise some spice will migrate to the aqueous if the ph is too low.
 
deweeb
#5 Posted : 2/4/2010 6:14:10 AM

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etherealsamba wrote:
my guess would be that since you used pre chilled water, it might have messed up things.. reason being, the water is cooled directly with refrigerant, which is freon..

Smile might be a problem people should be aware of..


Negative , the water is actually cooled in the lower rear portion of the fresh food section .The water enters the cabinet through a line that goes directly to a holding tank or remains in many feet of coiled plastic tubing . At no time is the water ever exposed to freon . All refrigeration systems are closed loops, if they weren't the freon would just dissipate into the atmosphere . So no worries about contamination .
 
 
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