My first extraction of san pedro

[NamRa]

Hello.

Today I am to start my first real extraction.
I have waited for some glassware to arrive and then I cleaned everything.
I am ready

I am using the ucidLemonade's sunflower oil mescaline extraction tek.

My question is.

When adding the lye to the water and adding this mixture to the cactus, is there a PH value I should be aimming for ??
I have a great PH meter I could use

 

[NamRa]

Well I have started.

I used this NAOH and I mixed it with the cactus poweder and added water.
I was wearing gloves and safty goggles, yes
Then I added more and more water and placed all from the sink to the magneteic stirrer/ heater.
I took a PH reading and it showed 10.8.
After adding the oil I thought it would be good to let the stirrer stir.
After I poured all over to a erlemeyer flask and put heater on a nice warm temp.
i am 20 min in and there is no sepperation at all.

Is my naoh ok ?
Did I stir the oil to much ?
Why is there no sepperation ?

 

[NamRa]

Need to work on my picture edit and upload skills

 

[endlessness]

Was the whole thing warm as you added the oil? Oil + mixing well with NaOH solution (particularly if warm/hot) = possible saponification...

So I think it might prevent layers from separating. I havent tried this tek myself but thats how you make soap, mix lye with vegetable oil.. it seems people make it work with extractions if its fast and cold, but if they take too long or its warm, saponification might happen,

In any case Im not sure if thats your case... Maybe others who tried this tek can give better feedback..

Mescaline has a pKa of 9.56 (the pH at which 50% of mescaline is in freebase form and 50% in salt form)

And if you use the freebase percentage calculator, at pH 10.8, it says 94.55% of mescaline would be in freebase form, so theoretically thats good... To improve yields maybe higher pH is better in some way but at the same time maybe it increases chance of saponification. Maybe better wait for someone who did the tek to give better feedback.

 

[NamRa]

Thanks for responding endnessless even if you are not familiar with this tek.

The tek talk about adding warm/hot water and thats what I did, maybe it was to hot.
I would like some help to figure out what went wrong

this morning everything was sollidified.
I maneged to get about 20 ml of oil seperated, its realy a dark brown oil.

I took half of the soap added a lot of water made it liquid and added more oil.
Now my kitchen is full of flasks with soapy water and still no clear seperation.
The erlemeyer has some seperation. It seems the oil is trapped between the watery and foamy layer

 

[endlessness]

Im sorry to say but I think youve just lost your extraction I think what happened is that the sunflower oil saponified indeed (hence why its hard), and now your mescaline is most likely trapped there... Maybe youre lucky that a bit of the mescaline is in that small amount of oil you were able to separate.. you can always try salting it out, and then re-a/bing if its too impure, to see if you get anything decent.

I am just about to add a warning to the sunflower mescaline tek so that people are aware that the pulls should be done within the hour or so.. Also this thing about adding the warm water, i understand warm water to help dissolving lye, but before adding the oil, I think it would make more sense if it had gotten cold, because then it will diminish chances of saponification.

The last thing I dont know, though, because Ive never done the tek, and this will take other people who have done the tek to say, is why it was so hard to separate the layers. Maybe it was too little water, or maybe one should do A/Bs and not STBs, or I dont know...

I hope it wasnt too much cactus you lost!! Keep experimenting, and thanks for sharing! Let us know if anything comes out of the small amount of oil...

 

[NamRa]

You are right Endlessness.

It felt like it was a lost cauze but today I tried with redesolving the soap adding water adding more oil, but it just became a inseperateble mess

I wish some of the more experienced could help me. I know a few I would like to pm but have to be patient for more priviliges.

I guess quite a lot of mescaline is in the tiny bit of oil. When I look at the pictures of the saturaded oil in the tek its quite yellow this one is dark brown.

Its possible I mixed to oil to much with my toy, the magnetic stirrer.

 

[mew]

wouldnt one be able to rehydrate this soap and bassify, let cool then add a different nps that like xylene *i dont use it* and mix seeing if any more nps could be saturated and removed from the mess.

 

[dg]

also have no exp using oil to extract cacti, but i would recommend a higher ph. (13-14)
more base is better ime, will break down the cacti to a runny liquid and aid separation
particularly if stb is the method

i always add water and base to cacti, blend on high (paint mixer on a drill...)
then wait until the sludge has fully slacked and turned to liquid before adding nps (10-24hrs)

 

[stolenface]

Ive done lucidlemonades sunflower oil tek myself- i followed the tek for the most part - added boiling water to the hydroxide/cactus mix but i also did my seperations in a hot water bath. I did 4 pulls back to back and everything came out fine. some pulls were yellow while others were dark red/brown. The darker pulls were on a batch where i added a lot more lye maybe 110 grams to 100g cactus, they did contain more mesc. than the yellow pulls. as for your dilemma i do not know how to come back from that sapponification , i did want to add that if you choose to do this tek again heat isnt all that bad as long as pulls are done quickly, the heat actually seemed to help.

EDIT: also to endlessness response about the water amount...100 mls of water to that much lye and cactus was not nearly enough, the first batch i started off following the tek but as i added the boiled water it was not enough to cause a nice reaction, i decided to eyeball it and what i beleive added was closer to 250-350ml's of water stirred and repeated 2 more times.the rest of the extraction was followed immediatley after this...4 pulls were done within 45 mins and every thing was fine.