Re-x to only remove the brown

[pete666]

no problem
dmt freebase is soluble in water. Not much, but to some degree yes. It is advised to minimize any unecessary water in the process.
low pH should not be a problem, as far as enough base is used later on.
has everything been dissolved in the non-polar before salting? Or the coloration appeared just after salting?
yeah, I don't think emulsion can appear just by temp change, without shaking

 

[tracid1987]

Everything has been dissolved in the nps before salting. i think the problem is with the vinegar, i wont use it anymore. but i have f*cked up the whole material. when i added NaOH the whole liquid became fizzy white. okay i dont know how it should look like, i kept adding NaOH slowly. i have checked the ph it was 11.7. then i have added more to get to 12.5 at least. checked. it was 11. how is it possible? i have added more and the ph became 10 and it became fully saturated by NaOH. Something gone too wrong. from ph 2.9 it went to 11.7 then back to 10. I have added NPS to pull but i think it was alredy too damaged because the NPS remained fully clear after pulling.

That was a lesson for me. but i still have to learn somehow from my own mistakes

 

[pete666]

When you add NaOH to the acidified water containing dmt salt, dmt turns into freebase, which is insoluble in water. So water goes milky .
Once you pull it with HOT naptha/heptane, it clears up. The non-polar clears up too
Why you saw slowly decreasing pH is a question. Maybe the reaction with vinegar was not immediate.
I can assure you that water saturated with NaOH won't have pH less than 14.
I never measure how much NaOH I add, I never measure pH at this step too. I just add enough, which is maybe 3 or 4 times more than necessary. No problem at all, high concentration of NaOH doesn't hurt anything, you cannot add too much.

 

[tracid1987]

It was so saturated i could not even dissolve any more NaOH. And i have a digital ph meter, it reads correctly. Strange that the nps remained as clear as before adding it to the solution-like nothing happened to it during stirring, turning the jar upside down. the pulling was hard because it was so saturated by NaOH that some cloudy looking transparent stuff has formed above the basic solution in the NPS. Just imagine you are looking out the window of a plane and you see the clouds everywhere. such cloudy but very transparent stuff reaching out of the basic solution into the nps. it was hard to do the pull because it was in the way of the pipette so i think i have pulled a little bit of it and thats not good because its full of NaOH. by the way i can see some crystals forming during precipitation but not much, i think i have fucked up the material or have to pre evaporate a bit.
Next time i will use something else instead of the vinegar.

We can close this topic, thank you very much for your time

 

[pete666]

So you've taken saturated non-polar, added about 5:1 (water:np) of water and added maximum possible NaOH and your pH of WATER LAYER is 11? You seem to have quite different physical rules than those in my reality

Anyway, no problem mate. Good luck!