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Minimizing oxidation during acetone redissolving? Options
 
tele
#1 Posted : 1/2/2012 10:00:03 AM
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Often the DMT before redissolving in acetone looks clearly whiter than after redissolving. I would guess this is due to long time exposure to oxygen?
If so, what would be good steps to minimize color change during this step? I guess using minimal amount of acetone would be one? How about fan drying to shorten the evaporation stage?

thanks
 

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endlessness
#2 Posted : 1/2/2012 10:41:58 AM

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I wonder how much of the darkening is actually oxidation of DMT, how much was already some darker spots that were hidden inside crystals that just got spread in a more visible way, or how much might be effects on color due to re-arrangement of crystals without actually having changed the content. Or maybe it is oxidation of other impurities around DMT. Or a mix of all of these.......

In any case, at least one thing you can do: Dividing your batch in 3 parts, one keeping indissolved, one dissolve in acetone and evaping as you do normally, and another evapping differently, later compare all the batches (picture/looks, description of smell, bioassay, etc..)

I think fan might make it faster but it might also make it oxidize more because of the amount of air/oxygen flow. I dont know how much this compensates for reduced time. Maybe the inverse would be better?

Are you evapping in the dark? Maybe that is also a variable to experiment with.

Whatever you try, let us know!
 
tele
#3 Posted : 1/2/2012 4:24:42 PM
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I've thought before that it's the small amount of yellow stuff mixed with the white, is what causes the general color change, however the amounts of slightly yellow stuff are so small that I wonder how it can create such noticeable color change. What I've always done though, is trying to keep the angel white colored always separated and redissolving it separately, which yields a more white product, but almost always looking slightly yellower than originally.
Yellow DMT is just as good, but I was wondering what's possible to be done. I'll try the darkness and see if it improves, I'll report if it's positive outcome.
I wonder if there are other substances than acetone that could take care of the removal of naphtha traces, and possibly create less yellow outcome?
 
DidMyTest
#4 Posted : 2/8/2012 7:13:50 PM

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Hmm I got a similar issue. Before I did the recrystalisation I had white waxy stuff and now it's more something orange. Additionally I have two questions
1) I couldn't see any impurities to discard when I dissolved it wether something yellowish nor the oily stuff at the bottom (like in the handbook), my solvent (acetone) was around 40 degrees C (Is this too hot).

2) It seemed to crystallize but there is still solvent left under the crystalls, I poked a whole throught the top layer (red marker).
Does this evaporate over time or can't it get through the layer?
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DidMyTest
#5 Posted : 2/13/2012 12:42:45 AM

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I dissolved around 2gr of DMT in 2x100ml Acetone (left picture) as you can see on the previous pictures the DMT was white but not crystalline more of a waxy consistency. After dissolving it in warm Acetone the solution is yellow (left picture) but there are no oils (even when cooled down to room temperature). I even reduced the 2X 100ml to 1x50ml and the colour of the solution got stronger but there are still no impurities (right picture). So

1) is it a solvent problem (--> using another solvent would help)?
2) Should I reduce it more because it isn't cloudy
3) Aren't there any impurities (maybe some complexes etc. which make the colour)
4) Cooling down should help EDIT: Makes it cloudy with some particles in it but still no oily stuff on the bottom nor a colour seperation.
?

I really would like to get maybe unhealthy impurities out of the final product...
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endlessness
#6 Posted : 2/19/2012 9:19:20 AM

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You need to read again because recrystallization is not done with acetone. Recrystallization as youre trying to do, is only done with naphtha/hexane/heptane. DMT and impurities are too soluble in acetone therefore you just dissolve them all, even if you reduce to small amount. Check the FAQ for instructions.

Acetone is only used to redissolve crystals and re-evaporate them because it helps getting rid of solvent traces trapped inside crystals, but thats the only thing it will clean, not any of the color.
 
tele
#7 Posted : 3/17/2012 12:09:43 PM
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I have noticed several times, that after the redissolved crystals are stored(Airtight container), they change color very noticeably after about three days, and when they are in crystal form, it takes weeks of months for the same amount of color change, does anyone have any thoughts why is this?
 
endlessness
#8 Posted : 3/17/2012 12:14:20 PM

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Maybe the type of crystals formed when redissolving in acetone have a formation that exposes more of the dmt to the air and therefore oxidises faster, while the crystals formed with naphtha crystallization are more "tucked in" and expose less of it to the air (maybe also why it traps more solvent...) ?

Do you keep it in a cold dark place? If not, u def should Smile
 
tele
#9 Posted : 3/17/2012 3:22:39 PM
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endlessness wrote:
Maybe the type of crystals formed when redissolving in acetone have a formation that exposes more of the dmt to the air and therefore oxidises faster, while the crystals formed with naphtha crystallization are more "tucked in" and expose less of it to the air (maybe also why it traps more solvent...) ?

Do you keep it in a cold dark place? If not, u def should Smile


thanks.

I keep dark n airtight but not cold... Just room temperature. I don't want to put my stash to the fridge or freezer.Smile
 
DudeMeetTyler
#10 Posted : 12/23/2012 2:55:43 PM

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Hey there,

Just wondering if there was been anymore development on this?

I just did a recrystallization which yielded some very nice white precipitates which contained a small amount of yellow specs throughout.

I then proceeded to dissolve the precipitates in acetone and let evaporate.
The result was a product that is a pale yellow.
The colour does not concern me, I am just curious about the reasons behind the colour change and if it is avoidable. There is just something about snow white products Smile

Thanks Smile

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