Pink/orange aqueous mescaline reduction PICS

[Binary Drool]

Process:
2ft san Pedro chopped and blended..
Boiled 3x and reduced, filtered and reduced again to 250ml.
Based with NAOH shaking accordingly over for 2 days.
Added 1:1 ratio of Xylene shaking accordingly for 2 days
Isolated Xylene and added 100ml 1% sulfuric acid solution shaking accordingly for 2 days.
Separated aqueous solution and am reducing to ~25ml at mild temperature.(Just steaming)

The one photo is when it began to bubble, the temperature was adjusted to where it is only steaming now.

I understand this yield will need to be purified, but has anyone ever gotten this pink/orange color solution? could it be from the type of acid I used?

Thoughts?

 

[Binary Drool]

25ml air drying

 

[The Day Tripper]

I'm excited lol.

Nice process BTW ☺

 

[Binary Drool]

Soo.. very minimal Xstal growth on the outer edge. You can see in the two bottom images.. but this seems to be highly unpure. this sludge like syrup will probably take a while to dry up. I will post pics of the dried powder.

 

[endlessness]

Let's see what comes out.

If chemicals used are pure, you should be good.

I never used sulphuric acid for mesc extraction, but from what I understand it won't evaporate off so any excess will be in your final product, and it can be yellowish oil. So it's important to titrate it properly, not sure if the dilution you used is appropriate. Do you have a pH meter? Pulls should be pH 6.

I've had pink/orangeish mesc before, but it was HCl. I re-a/b'ed and it came out perfect white crystals. So I suggest if you're not happy you can re-a/b and next time be more careful with the acid amounts.

 

[dg]

likely far to much acid for 2' of cacti

 

[Binary Drool]

Yes I used a pH meter and it was in the low 4 range. I was unaware that 6 was ideal. I used vinegar for my last extraction and was pretty happy with the results but I had some sulfuric acid and wanted to try it. I will post pics of this once fully dried and scraped up.

I think I will do another a/b.

strange how the aqueous solution was orange pink and now drying has turned to what looks like i spilt some pepsi on a pyrex dish.

I can see little needle crystals accumulating in the 'syrup'. I put a fan on it this morning.

 

[DansMaTete]

In my tiny experience (3 or 4 extractions), the lower pH gives the more brownish x-tals as others alkaloids are extracted.

 

[Binary Drool]

Here is a pic of my last extraction. Q21Q21 dry tek. 1:1 vinegar/water for acid.

Look how clear the aqueous solution is and the extract(400mg) still was far from pure.

 

[xram]

Maybe try to freeze precipitate the reduced aqueous solution (mix 50/50 with acetone and throw in freezer?). The excess acid may cause trouble, but perhaps it's worth a shot before you redo?

Generally, it's probably not a good idea to use this non-volatile acid if you're planning to evap the whole thing, because any excess will not evaporate (unlike with HCl).

 

[Binary Drool]

I think I will wait for this to dry up until I can easily get it all into a 100 ml beaker and dissolve in a 25ml NAOH mix. I will set this on the magnetic stirrer for a couple hours and then add 25ml Xylene letting it still mix for a couple hours. I will separate and remix in a 25ml .05% HCL solution and mix for another couple hours and then dry with a fan. I will never use sulfuric acid again.

 

[Binary Drool]

This morning the solution seemed to be at a stand still. It didn't evaporate much from last night. It was to wet to scrape up too, so i added ~120ml of hot water to the dish and redissolved. This is now in a 100ml beaker reducing to 25ml. strange how it took on this amber color. (yes, i know my hot plate could use a nice cleaning)

 

[dg]

I think I will wait for this to dry up until I can easily get it all into a 100 ml beaker and dissolve in a 25ml NAOH mix. I will set this on the magnetic stirrer for a couple hours and then add 25ml Xylene letting it still mix for a couple hours. I will separate and remix in a 25ml .05% HCL solution and mix for another couple hours and then dry with a fan. I will never use sulfuric acid again.

but sulfuric is the best once you get the hang of it!

for now you could dissolve impure crystal in a drop of 5 of water, just be sure it is completely dissolved.
reduce the volume a little bit
add acetone and put in freezer
filter pure crystals from the liquid

much easier than an all new A/B

 

[Binary Drool]

for now you could dissolve impure crystal in a drop of 5 of water, just be sure it is completely dissolved.

drop of 5?

do you mean .05%hcl?

 

[endlessness]

I think he meant drop or 5 , just pure water.

 

[Binary Drool]

right! haha

 

[Binary Drool]

Rather than add a few drops of water I wanted to base again and redo because I want to move away from this acid. EXTREMELY over acidified. I have never seen a reading this low on my pH meter. yikes. I based with NAOH back to 12 and brought this aqueous solution up to 300ml+ and added more Xylene. as you can see from the picture this lower aqueous layer is far from clear and the top NP layer is actually pretty clean. I'm going to make a .05%HCL solution tomorrow and go back to air drying. Will post pics. This experience has turned me away from sulfuric acid..

dg? why do you like it?

 

[dg]

like it because of purity, pretty glass clear crystals

just be careful not to over acidify and you're golden

 

[Binary Drool]

So re based and made a 20ml HCL acid solution at 5.5pH.
Obviously from this pic you can see the solution is pretty darn clear. I feel like most of the goodies are still in the NP layer. Here is what I got from the 20ml evap. hmm... I still have the xylene. I think ill go down in pH a bit and do another.. anyone have a specific pH suggestion?

 

[DansMaTete]

The pH at 5,5 is after pulls ? Because if xylene is really loaded, it can rise the pH. I check the pH after and going under 6 won't give more mescaline but other alkaloids.

Did you process more than one pull with the HCl solution ? I use to do 3 (the third is more to be sure cause 2 usualy are enough)