The Minimalist’s Mescaline Microwave Assisted Drytek

[JuremaSpaceship]

I just wrote all of this down in my notebook! I'm very excited to give it a try when I finally take cuttings from my trichs I have growing. I have 0 experience with mescaline but I'm confident that I can pull this off. Thank you for this!

 

[Korrupt]

I failed with this extraction method. I dont know, if i made some errors, or my cactus didnt contain any mescaline.
I have used 28 gram cactus powder, added some water to it, there wasnt excess water, just as much it could absorb, and ive added 1 gram citric acid to it, then cooked some. After i have added Ca(OH)2 to it, around 50g, then around 80g dried MgSO4.
I dont know how dry it should be at this point, it was a little bit moist. After these i have added dry acetone to it, and pulled it, and titrated with CASA. There was a very small amount of precipitation, but it was unmeasurable, maybe a few mg-s.
Its worth to evaporate the acetone, it could contain mescaline, or my cactus didnt contain any of it?

 

[starway6]

on the first post abovre instructions says......




Cactus Drying
Dried cactus ground to a powder in blender
Water added ...????:?:


back when i struggled to extract from slimy cactus pulp.. i learnt that drying cactus is a wast of time ...if your going to add water later...

I just grind it up into a mush but dont waste time drying it first...

you may want to skip drying the cactus into a powder...save time..

 

[Loveall]

Thanks for this TEK.

The pH Down I'm finding has phosphoric acid instead of sulfuric acid. A few posts ago it was mentioned that phosphoric acid also works. Does anyone else have experience titrating freebase mescaline in acetone with phosphoric acid? Phosphoric acid is also available at my local brew shop 8)

I'm thinking of trying this:

1) Cut fresh cacti and keep in a cool dark place for a week or two. Replant the tip.
2) Blend cacti with excess Ca(OH)2 and minimal water to make a paste
3) Dry paste in oven at low heat
4) Extract with dry acetone
5) Tirate acetone with phosphoric acid
6) Allow to settle/cristalyze in fridge overnight. Repat step 5 to verify no more clouds form.
7) Decant, rinse crystals with dry acetone, and dry.
8 ) Repeat steps 4) - 7). Use M1^2/(M1-M2) to estimate max yield and p = 1 - M2/M1 to estimate pulls needed to extract 90% of it.

This will be my first attempt at extracting mescaline. Feedback welcome.

 

[AcaciaConfusedYah]

Hey Loveall, and all!

It's been a while since I have visited this thread. It was written at a different time in my chemical explorations, and in the modern day, I would change many things.

I have not tried the procedure with phosphoric acid (at the time which I purchased the "pH Down for Ponds," the labeling on the product said that it was sulfuric acid. This may have changed over the years.) So, I am not certain if phosphoric acid would work. I liked the idea of sulfuric, because mescaline sulfate will freeze precipitate in acetone, even if there is water present. This reduces the need to make excess dry acetone. It's still important, IMO, to have dry acetone when doing the pulls from the plant matter, because excess water will pull ions, too. I do not know how phosphoric acid would perform when freeze precipitating from acetone and water.

As for your procedure, I would make one suggestion - probably not a great idea to add excess heat once the mescaline has been converted to freebase. I am unsure of the stability of freebase mescaline when exposed to heat, but mescaline in the salt form is relatively stable - more stable than many of the other alkaloids.

I did make sure to use anhydrous magnesium sulfate to dry the cactus mix, but i didn't use heat during the drying part, only the initial acidification. Removing the water from the mix will reduce the ions that may get pulled.... due to water being miscible with acetone.

Everything else (that you mentioned) seems like it is worth giving a try! If there is some information that supports mescaline's stability, as freebase, when exposed to heat, then you may be able to dry in the oven, but I've not looked into it..... yet.

Take Care!
ACY

 

[AcaciaConfusedYah]

Opps, had to edit a few things...


I added the SDS of the product that I use. It claims sulfuric. I wonder if the phosphoric acid is utilized in a different pH down product? From being in the fish industry, I do know that they use phosphoric acid as buffers, but they tend to avoid using them in conditions that would increase algae growth. Phosphate is a leading cause to excess algae growth, and a pond is in the open sun. Receiving excess light, and nutrient, algae will grow.

They use phosphoric acid based buffers in some products that are intended for aquariums that are in the house, and have low lighting. I.e. A phosphate buffer, in a tank that has high lighting requirements, will often result in the excessive algae growth unless all the nutrients are balanced and utilized by live plants.

 

[AcaciaConfusedYah]

on the first post abovre instructions says......




Cactus Drying
Dried cactus ground to a powder in blender
Water added ...????:?:


back when i struggled to extract from slimy cactus pulp.. i learnt that drying cactus is a wast of time ...if your going to add water later...

I just grind it up into a mush but dont waste time drying it first...

you may want to skip drying the cactus into a powder...save time..

Heh. Yeah, I had dried it to gather information about the dried biomass. I wanted to be able to provide some data that would result in the ability to gauge the amount of dried cactus to use, and the fresh pieces were too heavy for the scale that I have.

So, the dried part was to propose an option for folks who had harvested a cactus before they were intending to use it. Many folks dry the cacti to preserve it for a later date.

The re-hydration was used to gain an approximate amount of water needed to rehydrate the plant material enough to go through the acid cooks in the microwave. If the mescaline is in salt form, then it is much more stable. The acid plus the microwave will destroy the cells of the plant, and make mescaline more readily available for extraction.

I had anticipated furthering this tek, and going straight from fresh cacti, with out drying, so that people with fresh material could approximate the conditions needed to efficiently convert the mescaline to salt, and then be readily soluble in an aqueous phase. This would allow the "mix" to have a higher percent of attainable mescaline through lysing cells and converting to the soluble aqueous phase.

The mescaline will be in the aqueous mix, and when the Ca(OH)2 is added, it can readily convert to freebase. That would make it more attainable than trying to do all these procedures while the mescaline is in the cell.

I state that the mix should be dried before pulling with acetone.... Avoiding slime was not the purpose of this step, but a happy accident. I've never dealt with a slime when approaching cactus like this..... I have approached slime when I've tossed some fresh chunks in the blender and let it rip. Yeah, that was a pain in the ass. That's another reason that I dried first, then pulverized, and only rehydrated the material with a minimum amount of water.

But, it sounds like you're doing a completely different procedure. Thanks for the questions.

 

[AcaciaConfusedYah]

I failed with this extraction method. I dont know, if i made some errors, or my cactus didnt contain any mescaline.
I have used 28 gram cactus powder, added some water to it, there wasnt excess water, just as much it could absorb, and ive added 1 gram citric acid to it, then cooked some. After i have added Ca(OH)2 to it, around 50g, then around 80g dried MgSO4.
I dont know how dry it should be at this point, it was a little bit moist. After these i have added dry acetone to it, and pulled it, and titrated with CASA. There was a very small amount of precipitation, but it was unmeasurable, maybe a few mg-s.
Its worth to evaporate the acetone, it could contain mescaline, or my cactus didnt contain any of it?

Dang, I wish I had seen this sooner. Feel free to PM me if you have specific questions about a tek. I do not have the notifications set to send me an email when a post has been added to the thread.

You may have gone a little heavy on the citric acid, it doesn't take much. After some more experimenting, I found that it takes very little, actually.

I did not favor the CASA approach as much as I favored the sulfuric acid approach. Mescaline citrate is less likely to adequately precipitate in the presence of water. The acetone and the cacti mix would have needed to be REALLY dry, and then you'd have to take more precautions during the pulls and the filtering. Due to the miscibility of acetone and water, and the evaporation effect of acetone, the mix will become colder than room temperature, and will pull atmospheric water into the acetone. Since mescaline citrate is more soluble in water/acetone than mescaline sulfate, I tend to only use citric acid during the acid cook steps. After that, I use dried acetone for the pulls, but directly titrate sulfuric acid into the acetone. After that, I freeze precipitate, filter, collect, and then titrate some more sulfuric acid into the remaining acetone to see if I missed anything.

If there are no signs of precipitation, then I will evaporate the acetone, but be aware that acids like fumaric and citric will form crystals (if in excess) when the acetone evaporates. Therefor, your final yield may be contaminated with acid from the CASA or FASA. Sulfuric is more forgiving, requires lower amounts, and does not leave the same kind of residue upon evaporation-- well, you won't even need to evaporate it....

 

[Loveall]

Thanks ACY, makes sense. The aquarium product you pointed to is available, my bad I could not find such an example before. Thanks.

 

[AcaciaConfusedYah]

No problem! I hope that can clarify a few things.

I would love to see how the procedure worked out if using phosphoric acid. It may be worth experimentation if anyone has excess cactus and a little phosphoric acid.

I am unsure of the "freeze precipitation" process of mescaline phosphate. There have probably been some folks who have tried it. If mescaline phosphate can be freeze precipitated in the presence of water, then that would be an excellent addition to the collection of ideas that build this tek/thread. This thing is a growing and developing concept.

I just happen to be the person who wrote one of the ideas on the forum. I had pictures, but it seems that the original site that I had used to embed the images no longer exists.

There are a ton of variations that could be used in substitute for a specific part of the procedure, but we won't know until we try.

I tried benzoic acid. I was not really impressed. It "may" have worked (I never got the sample analyzed, and I still have it), but not really the same results that I have seen with sulfuric. If phosphoric works, then that would be really neat!

If you do decide to give this method a shot, share!

 

[Loveall]

I do have phosphoric acid from the brew shop. It's 10% (similar concentration to the aquarium sulphuric acid). I can try it in a subset of the acetone pull volume depending on how things go (I do want to follow the standard sulfuric acid salting path first).

There is something neat about simply using epson salt, lime, acetone, and phosphoric acid (an acid also in some sodas :surprised).

The cactus has been cut (tip removed for future replanting) and literally "chilling" in the garage. It will be there for a few days before I extract. Will let you know how it goes. It's only 7" , hopefully enough for a good introduction to a mescaline virgin like me

And again, thanks for writing down the TEK and answering questions. It's my personal favorite of the ones I've found and read.

 

[Loveall]

ACY, based on what you said about cell lysing, and since I'm skipping the acid microwave lysing, I'll let the cactus sit in the the Ca(OH)2 overnight. This should do some cell lysing. From this:

Alkaline Lysis
In alkaline lysis, OH− ions are the main component used for lysing cell membrane [37]. The lysis buffer consists of sodium hydroxide and sodium dodecyl sulphate (SDS). The OH− ion reacts with the cell membrane and breaks the fatty acid-glycerol ester bonds and subsequently makes the cell membrane permeable and the SDS solubilizes the proteins and the membrane. The pH range of 11.5–12.5 is preferable for cell lysis [3,38]. Although this method is suitable for all kinds of cells, this process is very slow and takes about 6 to 12 h.

For our purposes we will use lime instead of lye and skip the use of a detergent (SDS). The update to the original plan is that we will let the lime/cactus slurry stew overnight so (hopefully) the OH- ions work for us.

Also had a question about drying with magnesium sulphate. Did it lower the pH? I believe epson salts are slightly acidic. Maybe it does not matter in the end.

I'll be using the oven at low heat (170F) to dry the cactus lime slurry, hoping the mescaline FB is not affected negatively.

In short:

1) Cut fresh cacti and wait (hoping for mescaline buildup over a few days)
2) Blend cacti with lime/water to a slurry and wait (hoping for cell alkaline lysing over a few hours)
3) Dry over low heat
4) Pull with dry acetone
5) Add a suitable acid to crash mescaline salts

Seems simple enough. Hope it works out.

 

[AcaciaConfusedYah]

Yep! Cells can be lysed from alkaline conditions, as well. That's what a lot of people are relying on when they do a STB TEK. The only difference, that I considered, was that the mescaline salts were more soluble in an aqueous solution, so I rationalized that lysing the cells + acid would insure that more mescaline was available, once converted to FB once it was time to add the base.. However, I bet lysing in the calcium hydroxide will probably be fine.

Funny thing.... I actually was curious about the pH that would occur when using deionized water and the dried cacti. After a freeze/thaw and then a light heat bath, overall about 48 hours of sitting time, the pH was almost 8.0! lol I think it was 7.89.... so, the mescaline is pretty alkaline.

I am not sure about the pH of anhydrous magnesium sulfate - it may have some interaction with water and form very low amounts of sulfuric acid, or an intermediate, but I never noticed any issue when I had used it in my experiments. That's a good question, though. I'll take a little time, this evening, and look into the affect of mag sulfate in an "aqueous" solution. I don't think it will change anything about the composition of acetone, aside from removing water.

So, if the mag sulf is a little low, maybe the cacti being slightly high will counteract???

If you can, maybe take a small amount of DI water, and dissolve a mol of anhydrous magnesium sulfate and check the pH before and check the pH after. See what happens.

 

[Loveall]

Ok, here goes nothing.

1) First picture: 279g of fresh cut cactus that was left in the garage (~60F) for a week in a paper bag. No water loss noted (no change in weight)
2) Second picture: spines cut off and chopped up cactus in blender
3) Third picture 70g of lime blended with cacti. A beautiful runny light green liquid results (not viscous or syrupy). pH measured at 12.3.

So far this has been 10 minutes of work. Blended alkaline soup is going to rest overnight, hoping for OH- cell lysis.

Will post another update tomorrow.

 

[Loveall]

I am not sure about the pH of anhydrous magnesium sulfate - it may have some interaction with water and form very low amounts of sulfuric acid, or an intermediate, but I never noticed any issue when I had used it in my experiments. That's a good question, though. I'll take a little time, this evening, and look into the affect of mag sulfate in an "aqueous" solution. I don't think it will change anything about the composition of acetone, aside from removing water.

So, if the mag sulf is a little low, maybe the cacti being slightly high will counteract???

If you can, maybe take a small amount of DI water, and dissolve a mol of anhydrous magnesium sulfate and check the pH before and check the pH after. See what happens.

I went ahead and did a quick experiment to try to understand what the MgSO4 could do when using it to dry the alkaline cacti paste.

See image below: Dissolved .66g of Ca(OH)2 in 50ml of water: pH measured at 12.26. Adding MgSO4 in increments, the pH dropped slowly until about the ~1.6x0.66g mark (interestingly this is where the molarity of Ca(OH2) and MgSO4 dried at 450F is roughly the same I think). There is an abrupt change in pH there, down to pH~10. As you know, we don't want to be that low since it is close to the pKa of mescaline (9.77).

In my mind this means that Ca(OH)2 is combining with MgSO4 to give CaSO4 (another drying agent) and Mg(OH)2. If the lime is used up, the weaker alkalinity is given by Mg(OH)2.

Caveat is that this is under excess water conditions (worst case). In low water conditions things could be different.

What I think this means for the TEK: to play it safe, keep the MgSO4/Ca(OH)2 weight ratio below 1.5 while the paste is wet. Under these conditions the pH should stay two units above mescaline's pKa, which will result in the dry mescaline being (essentially) all in neutral form so the acetone can pick it up. It is OK to go above that weight ratio after the water is gone (and maybe when there is only very little water left). Only risky part is if there is too much water and/or too little Ca(OH)2 to begin with. In practice, if the paste is not dry yet and one has gotten to MgSO4/Ca(OH)2 mass ratio of 1.5, simply add more Ca(OH2) so more MgSO4 drying agent can be added while keeping the mass ratio at below 1.5.

 

[Grey Fox]

Loveall do you recall how large that cutting was in terms of inches? Did you grow it indoors under lights?

I am interested to see what the yield is. Thanks for posting.

 

[Loveall]

It is a 7 inch cutting. Grown outdoors until the first frost a couple months ago, then indoors by a window.

Cheers.

 

[Grey Fox]

Thanks for that info. Best luck with your extraction. :thumb_up:

 

[Loveall]

Ok, here goes nothing.

1) First picture: 279g of fresh cut cactus that was left in the garage (~60F) for a week in a paper bag. No water loss noted (no change in weight)
2) Second picture: spines cut off and chopped up cactus in blender
3) Third picture 70g of lime blended with cacti. A beautiful runny light green liquid results (not viscous or syrupy). pH measured at 12.3.

So far this has been 10 minutes of work. Blended alkaline soup is going to rest overnight, hoping for OH- cell lysis.

Will post another update tomorrow.

Alright, so after the overnight alkaline lysis (or the hope that it happened), completed the next steps (pictures below):

4) Poured the blended lime/cacti onto a shallow pan
5) Dried at low heat in the oven
6) Put dried material in jar and pulled with acetone
7) Filtered acetone and added 9.6% sulfuric acid. Cloudiness appeared, then a fine sediment.
7' ) A small sample of acetone was separated and to that phosphoric acid was added (10%). At first nothing happened as mentioned in chat, but after putting this in the freezer crystals formed.

So it looks like we are getting some mescaline salts. Will update again tomorrow, hope to have some yield numbers by then.

 

[AcaciaConfusedYah]

Great work, Loveall!

Thank you for adding these contributions to the tek. It may be that the mescaline phosphate is a viable option for folks who do not have access to sulfuric.

An additional option, to boost the pH, is to add a small amount of NaOH. The cacti mix can still be dried with relative ease, and it doesn't take much.

So, I am wondering if we had variations in how we used the anhydrous magnesium sulfate. I had allowed the cacti/Ca(OH)2 mix to come to near dryness before even adding the magnesium sulfate. So, with less water present, there may be less of an exchange between the proposed calcium sulfate and magnesium hydroxide. Magnesium hydroxide is very poorly soluble in water, worse than calcium hydroxide.

When I'd add the mag sulfate, it was almost already dry, and there was minimal (noticeable) hydration and dissociation. At which point are you adding the mag sulf? When it is still relatively wet? Or is is mostly dry?


Thanks!
ACY