No reaction when basifying. Help please.

[sicknastyboobear]

My friend is extracting acacia confusa and following this tek: http://www.howtogrowbud.com/tutorials-on-how-to-grow-bud/how-to-make-dmt/
There seems to be no reaction when basifying the acidic extracted liquid. He has followed the tek very precisely. When he adds the NaOH and water mixture to the acidic solution nothing seems to happen. The tek says the jar will heat up because the alkaloidal salts are turning into a freebase and the solution will turn gray and resemble a thick gel. None of this happens. It goes from a pH of 2 to a pH of 12 without heating up or changing in appearance.
Currently evaporating some solvent to see if there is any product.
Unless there's something he's missing, the only issue I could think of is that there is no dmt in the AC root bark that he has. Thanks for reading this and please help me if you can. :?

 

[treeshakers]

what's your basified solution look like? dark and sorta black?

is your naptha milky at room temp/in the fridge?

 

[wearepeople]

It sounds like you'll know pretty soon.

Let us now what happens with the evap!

 

[Kash]

If you describe everything you did for the extraction, then we could help you out.

 

[sicknastyboobear]

what's your basified solution look like? dark and sorta black?

is your naptha milky at room temp/in the fridge?

The solution is very dark purple or black. The naptha at room temperature was clear but in the freezer it is milky.

 

[sicknastyboobear]

Also what my friend did is as follows:
Ground AC root bark in blender until very finely ground. 30 grams per jar.
Point A: He then added 250 mL of distilled water acidified to pH of 2 to the root bark in each jar (shook well) and heated each jar in a hot water bath for 15-30 min.
After twenty four hours he filtered the RB mixture through a tea strainer and a cotton tshirt.
After that he repeated the process from point A two more times, allowing the mixture to sit for seven days each time instead of 24 hours (shaking the jars twice a day).
He then collected the liquid and filtered it through paper coffee filters.
After that he defatted the collected solution with naptha. Discarding the naptha and goop that was in it afterwards.
He prepared for basification by adding about 150 mL of warm naptha to each jar (Because the amount of jars was reduced, and there was liquid from 45 grams of RB in each jar).
Distilled water was basified to a pH of 12 by adding ~30g of NaOH to about ~600mL of water.
Basified water was added to the acidic mixture(of extracted liquid and naptha) until the pH was about 10. Then the mixture was stirred and turned.
No reaction was visible so one jar was basified further to a pH of 13 and the other 11. After no reaction was witnessed in two jars he stopped basifying the remaining jars to see what was going on. (No change in color, heat, or consistency)
After three days (because he went out of town) he isolated the naptha that had separated from the solution and attempted to precipitate in the freezer. Nothing was seen after several hours on its coldest setting so he is evaporating the solvent.

Can anybody tell me what went wrong or what is going on?

 

[null24]

So to my understanding, AFTER the defat stage (which I found unecc with ACRB) you added naptha THEN basified? I have not read a tek that goes in that order and not being a chemist dont see the reason for that. Everything Ive read goes the other way around: basify (til black heh heh) wait a bit then add your NPS. I just completed my first ever ext and had success of sorts by following thicklights tek outlined in the "having trouble ?) thread. I suggest poring over that, its been extremely helpful to a beginner like me. Good luck man, I feel ya.
Also it took alot longer to see results from freeze precip. Was your solvent milky? That is a sure sign that you have goods in there. Where (in the world) was the bark from? HA or Taiwan? was it brown or purple? It may be that yer bark isnt.
I used taiwanese for try no.1 with limited results but a batch from hawaii LOOKS better. More like purple MHRB.

 

[d*l*b]

The tek says the jar will heat up because the alkaloidal salts are turning into a freebase

An exothermic reaction happens when you add NaOH to plain water. If there wasn't a fast jump in pH you may not experience [much] heat on moving from acid to base.

the solution will turn gray and resemble a thick gel

The grey colour generally happens before the solution goes black. As you say your solutions is dark purple or black and is at pH 12 it should be fine.

you added naptha THEN basified? I have not read a tek that goes in that order.

You can add the non polar solvent prior to basifying only issue with that really is if the solution gets very hot on adding base you will pick up more oils.

 

[*oneironaut*]

what's your basified solution look like? dark and sorta black?

is your naptha milky at room temp/in the fridge?

The solution is very dark purple or black. The naptha at room temperature was clear but in the freezer it is milky.

hmmm... i had a similar experience with same vendor, although we're not talking about that since we don't talk about sourcing and vendors on the nexus....

 

[Kash]

What went wrong then? There are three possibilities I see here.

-You say that he shook the jar for 15-20 minutes and let it sit for 24 hours. This is incorrect. You want to shake the jar periodically every few hours. It wont extract nearly as much spice just sitting there undisturbed.

-You say your jars were pH 13 and 11. You cant go wrong with adding excess base here... go nuts! Make sure your solution is very basic pH 13-14.

-There is always the possibility that your starting plant material is bunk, but only consider that after all else fails to explain your results.

Also, your naptha may still very well have spice in it. If dmt is too dilute in naptha it will not crash out in the freezer. Try evaporating it to about 25% original volume then put in the freezer again. Best of luck!:thumb_up: