No - you have all the alkaloids dissolved in the xylene. You can discard the cactus tea at this point (but do not throw anything away until you are finished).

Now you put xylene and some distilled water in a container. The water will be slightly basic since there are alkaloids present, but they are much more soluble in xylene than in water.

By adding acid and mixing a little, the alkaloids turn into a water-soluble salt form and will be dissolved in water.

The water will stay basic as long as there is excess of unreacted alkaloids. Once you add enough acid, all the alkaloids will turn into salt form and move to water layer. The little excess acid will then make the water acidic.

Then you can discard the xylene and keep the water. Evaporate the water (the excess HCl will evaporate). You will be left with the alkaloids in salt form.

This process is called backsaling or back salting. It is the opposite of what you do when extracting, say, DMT - there you make the water basic to push alkaloids from polar solvent (water) to nonpolar. Now it's the opposite: You add acid to push alkaloids from nonpolar (xylene) to polar (water).

I think Fractalus understands, he was talking about HCl titration (back-salting), not the initial extraction from cactus slurry. He was just trying to say that he is (same as me) doing the initial extraction and titration together. If not, Fractalus, please correct me.

So he pulls xylene from cactus slurry (initial extraction) and does titration. When titration finishes, he puts empty xylene back to the cactus slurry and continues with next pull. Then with next titration.

Right?

I doubt you can do it like that. There is a lot of KOH, so you would have to add huge amounts of acid to acidify it. This doesn't seem like the right way.

But, if I understand correctly, you don't have any emulsion in the initial extraction. You pull the xylene out of the cactus slurry and the problems start when you approach pH 7 or lower while titrating, right?

If so, then I strongly suggest changing the np to toluene as a first solution trial to this problem. This is the way how I do it and it works.
If you don't have it now and you want to try something else, you can try titration to the point when the emulsion is not there yet. I would bet it starts to appear bellow pH 7, I think you've already written that. If you finish at pH 7, then most of mescaline is already transfered. I don't know exactly, but something like 95% should be in water layer. If you do first 3 pulls like that, you will have almost everything out in the water.
4th pull can be titrated to pH lower than 7, if you want to acquire all possible mescaline out of the xylene. You just have to stir VERY slowly, without any sloshing, just very gentle swirling. Then you could avoid the emulsion. Erlenmayer flask is the best for this purpose.
Well, in fact, when titrating just to pH 7, you get the most pure results. A lot of people are targeting this pH.
The only problem here would be the possibility of emulsion when you overshoot with the pH. And I would try to avoid it. I believe toluene might solve it for you.

When titrating, how much acid did you put there before it got to ph 7? How strong acid(%)? Are you able to calculate how much mescaline is there? If not, I can tell you how much acid is necessary for 1g of mescaline once I know this.

Here is the Mescaline HCl titration calculator

Thats exactly what he does!
after xylen back to cacti slurry, the jar mix good to saturate the xylen with alkaloid again and now the alkaloid xylen goes back to the same hcl water that he titrate before and repeat...
swim understand that when the xylen pulled back to the hcl water and the ph dosnt change it means that all the alkaloid are pulled, that is correct?!

thats correct, no problem with xylen/cacti, the problem begain when xylen pulled from cacti jar to new jar with dh2o and there the emulsion strat to form after mixing the the jar!

true!

faw drop of 2% hcl and 25 ml of water that will be about 3 ph, he dont calculate, just add enought hcl until its reached ph 7,
how can one know how much mesc there is in there before he extracted it?

I am doing 3 pulls, so 3 titrations. Every titration has its own water. After every titration the water is mixed and evaporated together.
If small amount of added HCl causes big drop in pH, there are little alkaloids in the solution.
I have uploaded titration calculator in previous post. Just enter how strong HCl you are adding (I am using 3,5%) and you will get mililiters of acid necessary for one gram. The more precise you are, the more precise the estimate is. I am usually +-5%
You are measuring how much acid you need to reach neutral pH

I see.

now the emulsion accured when swim mix the xylen with dh20 without even adding hcl in hot water bath...

Well, this situation is difficult. The main concern is to avoid emulsion in initial extraction. Which worked well. For back-salting with xylene and these problems I don't see other possibility than careful stirring without any sloshing. And this is much slower and much more labour intensive than proper mixing.
Again, I would try switching to toluene. Check this thread

so one should evap that alkaloid xylen and flush the remains with fresh toluene?

To salvage what you have now yes, evap xylene, but I would not use heat, just airflow, the mesc freebase isn't likely very stable.
For next pull(s) use just toluene. And pray

Is there any basis for the claim that toluene won't cause more emulsion than xylene?

I will use xylene this time as I have the bottle opened and lots of it ready for recycling. I don't want to open a fresh bottle of toluene.

As for the backsalting, just gently swirling the liquid is enough to salt alkaloids into the water layer. Inversion also helps, but there is no need for shaking.

I use nitrazie indicator which shows visually how the alkaline stuff protrudes into the acidic water, neutralizing the stuff

Okay today is the day D so starting the extraction and will report later this day

Okay first problems:

1. the amount of salt is HUGE (over 300 grams) - it refuses to dissolve in the soup, it's on the edge of solubility even if the water would be clear:

For 120 grams of cactus powder, your tek requires 840 ml water (120:840 = 1:7 ratio) and 180 g of KOH (120:180 = 1:1.5 ratio).

Then we add 180 ml water (120:180 = 1:1.5 ratio) and 313 g salt (120:313 = 1:2.61 ratio).

So we are adding over 300 grams of salt in little over 1 liter of water. This would be hard to dissolve completely even if the water is clear, but it already contains: 120 grams of cactus powder and 180 grams of KOH. Are you sure that much salt is okay?

2. the xylene refuses to separate from the aqueous and I have huge emulsion even without any shaking - the soup is not watery nor thick - I heated and stirred it several times for two extra days but it did not turn completely watery.

It seems the solution is already so thick it traps the NPS. I will wait some hours for phase separation but then probably dilute the soup as otherwise it would be hard to work with.

So far this Tek does not work for me at all

This is how it looks in the sep. funnel. The xylene forms only a thin layer (50 ml or so) even though I added 200 ml. Most of it is trapped in the soup.

Let's focus on the emulsion first, we can talk about the rest later.
How long have you left it still to settle after mixing? Have you been mixing it? For how long?

Mixing by gentle swirling and inversion for about 4 minutes, then left to sit for over 2 hours.

Now it looks like on the picture. After about an hour I swirled it very gently some more and the xylene layer got considerably thicker.

What is interesting, there are actually multiple layers.

So after draining, the layer right below the xylene is actually a HUGE emulsion.

I went for this tek to avoid dreaded emulsions but it seems to actually give worse results than typical A/B extraction.

Have you considered saponification? You know the plant fats will turn to soap in such high pH environment and soap makes bubbles, i.e. emulsion.

Maybe if your cactus was less fatty of you removed the waxy skin beforehand, it could work. But in my case I sttuggle.

For whatever reason it works for you, it must be in your specific technique. I am unale to reproduce it.

I am really sorry for this result. The first separation happens within one or two hours. It may be more, but never more than four. Next separations are faster. Have you left it separating in the funnel, or is it already drained? I don't know what was wrong in your case, but you could have it left for half day to ensure the emulsion won't disintegrate.
I would like to know what was Fractalus's entry material, his trial gave much different results. Did it contain waxy skin and core, Fractalus?
As I've written in the first post, I am using PT chips. The chips are just green tissue. I didn't try it with anything else. Anyway, I was planning to try it with complete cactus once I have it, so now it looks like very questionable path.
I never stirr slowly, it is always shaking without mercy. I doubt it is the problem here, but you can try to avoid fear of emulsions and shake this way. I understand it may to go against common sense, but I would do it this way.
And yes, I have considerecd saponification. But it never happened for me while extracting mescaline with NaCl.

I waited another 2 hours but only 10 ml of xylene resolved, the rest 90 ml stayed trapped in emulsion.

In the second pull, it's pretty much the same. I added 200 ml xylene and got only 100 ml back, the rest is lost in emulsion.

At least the emulsion layer is clearer. I will put in on a hotplate under slow stirring a low heat overnight. This often helps.

I don't know the source of the cactus. I have just been given the cactus tea with some estimate on how much powder has been used.

I am afraid there will be huge loss in yield. I will report back tommorow.