yes!
strange thing happend, a tiny water layer started to become from the emulsion at the bottom but its has no crystal color like before, it now clear...

ok the emulsion start to break really slow and strange thing there is dark yellow xylen(was dark greenish grey when pulled from cacti jar), the emulsion at strong smailey yellow like this and the water are clear color....

Ah ha. Okay I will heat it and stir occassionally for the next 2 days. I don't want to use blender as we use it for food and I found pouring the hot caustic slurry between pot and blender would be ... inconvenient.

I usually pull with xylene, add it to a sep. funnel along with distilled water and a drop of nitrazine indicator. Then I continually add 1% sulfuric acid with a dropper, shaking in between additions, until the indicator turns yellow (acidic).

Fractalus, weird, but as I said, every change to the procedure means danger of unwanted reactions. Obviously xylene is reacting somehow with something when the solution reaches acidic levels. I strongly suggest using toluene next time. It is prone to emulsion in the titration stage too, but only at room temperatures. When heated to 60C or more, there is no emulsion at all. The titration is fast, so such short heating is not pain at all. I am not using heater, just hot tap water bath.
In fact the titration could be done without measuring pH, if there is no need to know how much goodies is in the solution, because the color of np or water is telling everything. The np after initial extraction and separation has some color from the cactus. When titrating, as pH bellow 7 is reached, a lot of this coloring moves from np to the water. After few extractions one can say when this happens, so the desired pH has been reached. It is similar to titration of dmt.

So, with breaking the xylene, I can't directly help you, because I can't try it myself. Anyway, if you get to the point you don't know how to break it, just let me know, I can suggest what to do. Anyway, the description has to be better, in fact I didn't understand what you have written - what you did and in what state you are just now.

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This is really good technique.
I just don't have experience with xylene, so I can't know if there are going to be any problems with emulsions

blue.magic, you have quoted me, but that quote was for titration. Was it in error?
if you are reacting to the mixing (in initial extraction, not titration), then I didn't mean to mix it in mixer. I use mixer only for initial mixing. Then I have it in the glass vessels, enclosed, and I mix it few seconds by hands. If you have it in a pot, just use some stirring spoon
But heating it here is ok, speeds up the process

the emulsion breaking at slow rate in the 60-80 temp hot water bath...
now the emulsion/xylen is in bright smailey yellow color and the water is crystal color.

the whole titration part take much longer when swim sep funnel got broken...

swim cant upload picture at the moment for all to see but the xylen/emulsion is really banana yellow which is really wiered..anyone come acros somthing like this before?

any idea how to return the xylen/emulsion yellow layer to its normal state???
should swim put another 50ml or so of xylen in the cacti jar to pull alkaloid and then separete the alkaloid xylen layer and put it in emulsion jar to base the emulsion a bit more?

Fractalus, I have to understand what you did before I suggest anything.



I don't understand it. Does it mean you put the emulsion (everything from titration) back to cacti jar? Or just xylene? If just xylene, what xylene, if there was only one big emulsion (water and xylene mixed)?

Well, I think I understand you, you got just two layers - emulsion and xylene, right?

If so, then...
I would separate the xylene.
I would separate the emulsion.
Then I would break the emulsion (alone). Heat/time/vibration is the best solution. If it doesn't break up the emulsion, I would try to basify it by KOH. If emulsion breaks, I would take xylene and mix it with previously separated xylene and titrate it or use it for another pull from cactus jar. Water would go to cactus jar
If basification by KOH doesn't help, I would try acidification by HCl. If it breaks, water would go to cactus jar, maybe with some additional KOH. Xylene would go for next pull

Breaking up the emulsion should not be problem, the problem is how to avoid it for next titration

swim will explain how he got to this situation.
hes sep funnel broken letly so he has to pipete the water from the xylen/water jar.
he pulls the water, then add hcl until the ph is about 7, put the water back in the jar, shake it and repeat.
after the fifth titration pipeting an emulsion in banana yellow color start to form in the middle,
he keep titrating (not the smartest idea) and eventualy the water/emulsion become 1 emulsion layer.
so then there was 2 layers: one of xylen and one of emulsion that "swalowed" the water in yellow bright banana color.
then swim tought that it will be good idea to pull the xylen, put it back in the cacti jar to absorb alkloid and then return the alkaloid xylen to "base" the emulsion with the alkaloid...
unfortunetley the 2 layer of "basic" xylen and emulsion become 1 layer of emulsion...
so now there is one banana yellow emulsion layer that slowly breaking down by the hot water bath (60-80C) and a water layer with alkaloid start to form at the bottom with a mild emulsion between the hardcore emulsion and the water...

yessssssss!!!!!
finaly the emulsion disapear with lots of koh and everything goes back to cacti jar and prosses can continued!
thank a lot pete!!

Are we talking about titration? So at the beginning we have xylene with mescaline freebase (from initial extraction) and we want to transfer mescaline to water as mescaline HCl? I hope so

You say : "he pulls the water, then add hcl until the ph is about 7, put the water back in the jar". Why are you pulling water? To squirt it over pH paper? Or are you pulling it all? If so, why? Why are you putting the water back after addition of HCl?

Titration procedure simply : I have xylene with mescaline freebase. I add water. Then I heat it up to 60C. Then incrementally add a (calculated)bit of HCl, mix for few minutes, let settle, take sample (by pipette) of bottom layer (water), squirt it on pH paper and check pH. If basic, repeat. If acidic, finished - I can separate water layer and evaporate.
How is "he pulls the water, then add hcl until the ph is about 7, put the water back in the jar" related to this?

Please check you understand the titration first (my previous post), so you don't get to this problem with next titration.

If we are talking about separation after titration, there is no need of separation funnel...

I just use beaker for pouring off the solvent as much as possible. Then I use glass funnel with cotton blocking the output. I use turkey baster to take the bottom water from beaker (with water and tiny np at the top). Turkey baster is used, because I don't want any np to touch the cotton. Once the funnel is almost full, I release a bit the cotton by tiny wooden stick, so it starts to go slowly through. Then I slowly pour all the water+bit of np from the beaker to the funnel. The np stays at the top, so I am sure only water goes through. Once np should go through, I remove the funnel. Finished

anyway every time swim add hcl to the water/xylen he got emulsion...some minor some big but all emulsion...
he think that it must be from the fats and oils in the cacti as he saw it in many others teks,
how one's can defat in stb? can one's start to break the cacti cell with 1:7 water and koh like in the instruction and after he add the np to add lots of acid to ph 2 or so, then defat by adding np 50ml each time, shake, discard and stop when the np is clear, and then base again , and pull with xylen, do titration and evap the hcl water?

No, I am confused. This doesn't make sense to me. Please read this and tell me, whether it makes sense to you :

Titration procedure simply : I have xylene with mescaline freebase. I add water. Then I heat it up to 60C. Then incrementally add a (calculated)bit of HCl, mix for few minutes, let settle, take sample (by pipette) of bottom layer (water), squirt it on pH paper or pH meter and check pH. If basic, repeat. If acidic, finished - I can separate water layer and evaporate. Sample water is of course returned to the xylene/water mix after each pH check

Are you doing it exactly like that?
How much HCl do you add?

"If basic, repeat. If acidic, finished" ok so after acidic he pulls the xylen back to the cacti jar, then mix the cacti jar, pull the xylen back to the acidic water and titrate again and so forth...

and what about the defating stage??