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Just whipped up some DMT, right?

ah! the smearing does appear to work

I will report back with the latest batch, where I tightened the tek (I believe I did it perfectly this time)

*fingers crossed*
 
If you used too little NaOH you wouldn't have pulled anything.

I used 1 table spoon for 50g bark/600ml of water... so roughly 10g, which is why I believe this entire go has been a disaster.

This time I used 75G bark /750 ML water /50g NaOH
 
naoh 40 g/mol - 10 g is 0.25 mol
0.25 / 0.6 = 0.42 M
pOH = - log (0.42) = 0.38
pH = 14 - 0.38 = 13.62

Even with 10 grams on 600 ml you get a pH of above 13.5 ...
So no it seems you added enough...

Let me check a tek for proposed concentrations or pH to use for basification.
I see that the 50 g NaOH in 750 ml is exactly what the Noman tek says.

Then again, more lye can increase yield said here:

Right after this first extraction I wanted to see if increasing the amount of NaOH would increase the yield so 75 g more of NaOH was dissolved into ~750 mL of additional water and added to the mix with 400 mL more of naphtha poured into the bowl which was stirred again for close to 30 minutes and carefully separated from the mix for evaporation. With the amount of NaOH doubled the yield was found to be 50% greater at 1.5 g of alkaloid and because of this I recommend a minimum of 150 g of NaOH for 2 L of water when extracting 250–500 g of broken root bark and from 200–250 g of this base per 3+ L of water when extracting from 500–1000 g of broken root bark.

It is not as black and white as pulling nothing or everything like phuckingnuts seems to suggest...
 
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yeah...you're right it's not black and white exactly but once you cross that threshold you pull or you don't pull. After a while buffering action from hard water might cause you to add some more, and you can't add too much.
IME, though, once it goes from red to gray(thick gray soup) and then to black...it pulls...period.
The only thing that too little might do is create a more stubborn emulsion, but what separates even then will pull.
 
It is logarithmic. If the pKa of DMT is around 8.8 / just under 9 forgot the exact value, that means that at pH 8.8 there is 50% of the present DMT protonated (which will go into the watery layer) and 50% deprotonated (which will go into the naphtha). Go to pH 10 and the part left in the water goes from 50 to what, 5% ? Then to pH 11 it goes to 0.5% and becomes negligible which is I guess related to the reason why pH 11.2 is considered the golden number for the base step. At that point it should basically (no pun intended) be a full pull, if swirled properly etc of course.
In that previous quote someone reports better yields with even bigger excess of NaOH (not really the right term, it's not a reagent), but others report that above pH 13 the DMT becomes unstable.

I don't really know why such high pH is recommended by a lot of people, maybe part of the lye is lost on the bark somehow. No wait this is probably the reason: if you first do an acidic step and then add concentrated lye, you lose plenty of lye to the neutralisation. If you check pH after neutralisation (if that even applies to the tek you use) it is different and you should probably not aim for pH 13 at that point but around the 11.2 I mentioned earlier.

In that previous calculation I did not account for neutralised acid, sorry have not checked that. But I am checking really quickly now and see that it does not apply anyway since it is STB.

So maybe TS is getting those teks mixed up and the amount of lye each requires?
 
I go by color and smell...unscientific ?...yes...does it work...yes.
Do I get more in subsequent pulls with even more lye ?...no.
 
so, how long do you guys recommend on freezing for? It's been freezing since last night and this is what the dish looks like. There is still visible clear NAPHTA inside as well.

Zyfx97B.jpg
 
The rule of thumb, for me, is put it in the freezer, it'll cloud up. Wait till it clears, at this point all the DMT that is going to precipitate at that temp & concentration is there.
Take it out of freezer, pour off Naptha, dry crystals.
Evaporate remaining Naptha til it starts to cloud, put back in freezer repeat as many time as necssary.
 
The rule of thumb, for me, is put it in the freezer, it'll cloud up. Wait till it clears, at this point all the DMT that is going to precipitate at that temp & concentration is there.
Take it out of freezer, pour off Naptha, dry crystals.
Evaporate remaining Naptha til it starts to cloud, put back in freezer repeat as many time as necssary.

when I roll all the Naphta down into the corner of the pyrex, it's definitely got a visible cloudy, smogginess to it. I'll leave it overnight and check result in the morning.
 
upon further inspection, it wasn't cloudy at all. it was simply yellow. I poured the NAPHTA into another dish and they immediately began to solidify further,

these some beautiful crystals :)

Success!
 
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