Alternative to Recrystallization: No NP Solvent Needed

[gibran2]

I’ve never tried the following procedure in it’s entirety, but I’m wondering if it would yield clean spice?

1 --- dissolve 1g freebase in a minimal amount of vinegar
2 --- dilute solution to about 100ml
3 --- prepare a solution of NaOH: about 0.5g NaOH in 100ml water
4 --- add NaOH solution to DMT acetate solution
5 --- freebase DMT will immediately precipitate
6 --- allow DMT to settle, remove most of water via decanting or siphoning
7 --- rinse with dilute sodium carbonate solution to remove NaOH
8 --- allow DMT to settle, remove most of water via decanting or siphoning
9 --- repeat 7,8 to ensure all traces of NaOH are removed
10 --- allow remaining water to evaporate, leaving behind DMT freebase

I’ve never tried all of the steps, but have done steps 1-5 as part of a mini A/B to clean some really dirty DMT. The DMT that precipitates out seemd to be very clean and the solution became discolored from the impurities. I then followed up with a NP extraction, but have always wondered if the DMT could just be separated as-is without doing an extraction. Any thoughts?

 

[Phlux-]

suggestion - perhaps add a step where before separation one puts it in the fridge - to make the spice harder and colder and thus the water easier to pour off.
also choice of vessel could mean a lot here.

all would need to be tried tho - i didnt play with that separation enough - only when out of np

 

[Infundibulum]

I’ve never tried the following procedure in it’s entirety, but I’m wondering if it would yield clean spice?

1 --- dissolve 1g freebase in a minimal amount of vinegar
2 --- dilute solution to about 100ml
3 --- prepare a solution of NaOH: about 0.5g NaOH in 100ml water
4 --- add NaOH solution to DMT acetate solution
5 --- freebase DMT will immediately precipitate
6 --- allow DMT to settle, remove most of water via decanting or siphoning
7 --- rinse with dilute sodium carbonate solution to remove NaOH
8 --- allow DMT to settle, remove most of water via decanting or siphoning
9 --- repeat 7,8 to ensure all traces of NaOH are removed
10 --- allow remaining water to evaporate, leaving behind DMT freebase

I’ve never tried all of the steps, but have done steps 1-5 as part of a mini A/B to clean some really dirty DMT. The DMT that precipitates out seemd to be very clean and the solution became discolored from the impurities. I then followed up with a NP extraction, but have always wondered if the DMT could just be separated as-is without doing an extraction. Any thoughts?

This is more-or-less analogous to SWIM's approach some time ago, and endlessness run some nice tests showing that this comparison is very very adequate.

The only unresolved issue is that endlessness and few other people found that if sodium carbonate is added to freebase dmt-acetate nothing precipitates. But precipitates and the freebasing does form when dmt-fumarate is used! This is bizarre. You said that you've tried that already, no? So can you confirm that precipitates form when dmt-acetate is based with sodium hydroxide? This is indeed interesting!

Also, in the beginning of your post you say that you want to clean the dmt, but I am not sure how purer it will get by this method. Maybe more? The method of cleaning up depends on the suspected types of impurities present in the dmt. Maybe start from there; the (yellow?) discoloration you saw left behind after the water precipitation of dmt is maybe n-oxide that is considered more water soluble than dmt.

 

[gibran2]

The only unresolved issue is that endlessness and few other people found that if sodium carbonate is added to freebase dmt-acetate nothing precipitates. But precipitates and the freebasing does form when dmt-fumarate is used! This is bizarre. You said that you've tried that already, no? So can you confirm that precipitates form when dmt-acetate is based with sodium hydroxide? This is indeed interesting!

Oh yes – DMT acetate can be very nicely freebased with sodium hydroxide – when the NaOH solution is added, it precipitates so rapidly that it looks like you have a glass of milk.

 

[prottel]

Sodium hydroxide works nicely with dmt acetate. Instant milk.

 

[Gir]

I actually just did this not too long ago..

couldnt get my spice clean, was this ragged yellow.

so I dissolved it all in very hot vinegar (~100mL)

I heated it up because everything dissolves better heated. Once that was done and there were no floaties, it was a yellowish tinge, I added about 250-300mL water to raise the level and then added about 50mL of saturated naOH sltn. Immediately it started to precip. I finished pouring in my solution and stirred it around carefully.

I waited about 3 hours (starcraft..) and came back poof, there was precip at the bottom of the glass, it was in chunks. I siphoned and filtered and siphoned and filtered until I got the water level to about 15mL. I then left everything else inside the beaker to evap, and left my 2 filter papers to dry.

It worked very nicely and I was able to recover quite a bit of spice.

 

[gibran2]

I actually just did this not too long ago..

couldnt get my spice clean, was this ragged yellow.

so I dissolved it all in very hot vinegar (~100mL)

I heated it up because everything dissolves better heated. Once that was done and there were no floaties, it was a yellowish tinge, I added about 250-300mL water to raise the level and then added about 50mL of saturated naOH sltn. Immediately it started to precip. I finished pouring in my solution and stirred it around carefully.

I waited about 3 hours (starcraft..) and came back poof, there was precip at the bottom of the glass, it was in chunks. I siphoned and filtered and siphoned and filtered until I got the water level to about 15mL. I then left everything else inside the beaker to evap, and left my 2 filter papers to dry.

It worked very nicely and I was able to recover quite a bit of spice.

Without any rinsing, you might still have some NaOH mixed in with your spice. Be careful. (Or did you rinse during the siphon and filter steps?)

Also, how clean was the resultant spice compared to what you started with?

 

[DiMiTriX]

i just read it right now after swim did the same but putting it in fridge....very nice white clouds
he was thinking if he could basify with magnetic stirrer on and stop basification when clouds are stable..maybe just add few more lye drops? no need to do that but it's more elegant
it's similar to tirtration