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The Minimalist’s Mescaline Microwave Assisted Drytek Options
 
starway6
#21 Posted : 1/2/2016 1:42:43 AM

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AcaciaConfusedYah wrote:
The Minimalist’s Mescaline Microwave Assisted Drytek - MMMADtek
***entirety of OP quote removed by mod to keep all the massive pics from reloading every time the page is opened.***



Sounds interesting as ive never had much luck getting cactus to yeild near pure mescaline crystals..
Cactus extraction is messy and a pain in the ....!

But you stated above..your cacti was..[Trichocereus pachanoi monstrose.?]...isnt that two diferent cacti species? ...[Trichocereus Pachanoi] and Monstrose?
Were you using two types of cacti?

Also using a microwave is an idea ive always wanted to try.. concidering the microwave heats by rearanging the molecular structure of whats being heated during heating process.

Are you shure your final product doesnt have any non mescaline crystals in it?

Have you tryed your product yet?

If its reasonably pure mescaline crystals it should be a smooth beautyfull trip without almost any body load...

 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
AcaciaConfusedYah
#22 Posted : 1/3/2016 2:21:58 AM

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Quote:
Sounds interesting as ive never had much luck getting cactus to yeild near pure mescaline crystals..
Cactus extraction is messy and a pain in the ....!


Heheh, yeah some of the extractions can certainly be a messy endeavor. This one is mildly messy, but not too bad. With cleaning, crystals can be had!

Quote:
But you stated above..your cacti was..[Trichocereus pachanoi monstrose.?]...isnt that two diferent cacti species? ...[Trichocereus Pachanoi] and Monstrose?
Were you using two types of cacti?


It was a Trichocereus pachanoi var. monstrose. Monstrose is just a term that identifies that it is a mutant variation of the original Pachanoi. This just means that the ribs grow in funky patters, occasionally. But for the most part, it looks like a standard pachanoi. Some Trich pachanoi monstrose can actually be crested, rather than have the weird rib patterns. They are very pretty cacti.

Quote:
Also using a microwave is an idea I've always wanted to try.. concidering the microwave heats by rearanging the molecular structure of whats being heated during heating process.

Are you shure your final product doesnt have any non mescaline crystals in it?

Have you tryed your product yet?

If its reasonably pure mescaline crystals it should be a smooth beautyfull trip without almost any body load...


Yes, I have tried it, and it is mescaline. It was the strongest trip I have had from extracted mescaline, and only an unknown amount of resin has surpassed the intensity of the extract. Initially, i yielded a contaminated product, and had to clean it via dry acetone washes. That was using the fumaric acid. In later tests, using the Sulfuric acid, I received a much more pure intial product - that is why I have edited some of the original post to indicate that sulfuric is the preferred acid to use for titration. However, I have not yet tried my sulfuric. I plan to do so soon. I will certainly report back and share the results.

Very happy <3
Have a great day!
 
mitosis
#23 Posted : 1/6/2016 5:46:38 AM

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I've only tried a wet 5 gal carboy tek with naoh toluene and hcl, and had really good results my first try.

I've never used acetone to wash my finial product but have used distilled water to redissolve and re-evap to drive off excess HCl trapped in the crystal matrix of initial crystallization post salting. I've also used MEK+distilled water once to separate crystals from an amber goo yielded on a much smaller batch.

I understand this tek is dry and very different than the more common aqueous toluene methods.

My questions concerning your tek:
1)Why H2SO4? Why not NaCl? hydrochloric (muriatic) containing but not saturated acetone (or Methyl Ethyl Ketone ) I'm talking either a minimal amount muriatic (2-3 drops per rinse at a time unless its scaled up). I know muriatic contains water, but I'm uncertain that bubbling HCl gas through acetone will saturate it if that acetone is completely dry and contains no water.

continuing with that train of thought,

2)How might NaCl best be incorporated into your tek for those who prefer it as the acid used out of familiarity with a given expected acid to salt yield ratio?

3)Can MEK replace acetone in this tek?
 
AcaciaConfusedYah
#24 Posted : 1/9/2016 1:34:13 PM

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Quote:
1)Why H2SO4? Why not NaCl? hydrochloric (muriatic) containing but not saturated acetone (or Methyl Ethyl Ketone ) I'm talking either a minimal amount muriatic (2-3 drops per rinse at a time unless its scaled up). I know muriatic contains water, but I'm uncertain that bubbling HCl gas through acetone will saturate it if that acetone is completely dry and contains no water.


This tek is still most certainly a work in progress, and I hope that it inspires other people to try various different combinations of acid saturated Acetone for crashing the mescaline alkaloids.

So, the reason I chose sulfuric as the best choice, is due to the ability to freeze precipitate from Acetone/water mix. So far, Mescaline sulfate is the only mescaline salt that will still precipitate with the presence of water in the acetone. Mescaline citrate, fumarate, and HCl are going to be soluble in water, and will not readily crash out of the solution if there is accidental water contamination in the acetone.

Feel free to experiment!

Quote:
2)How might NaCl best be incorporated into your tek for those who prefer it as the acid used out of familiarity with a given expected acid to salt yield ratio?


Sodium Chloride is not something that I have experimented with in this tek. I see no benefit to using it at all in this tek. You sure you Don't mean HCl? Hydrochloric acid? If that's what you meant, then it might work. But the solubility issue mentioned above would be my reason to still choose sulfate - alkaloids will crash out of solution much easier.

Quote:
3)Can MEK replace acetone in this tek?


You could use it for the cleaning washes, for sure. As far as for an initial solvent - am not sure. I have not tried it, as acetone is much easier for me to obtain.
Have a great day!
 
Poekus
#25 Posted : 1/9/2016 6:53:50 PM
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I don't have a microwave ,but nice to see this NP free mescaline tek.

Why are you doing the acidic boil? Usually this is done either prior to defat to make sure al alkaloids are in salt form or added to water to let the alkaloids migrate from the tissue to the water in case of a tea based extraction. In your TEK immediately after the acidic addition, you basify and dry. I think the acid boil could be left out with equal results. Did you try this?

Also why did you dry the cactus first and than immediately rehydrate it in the next step? Why not putting it in the blender fresh and then in the microwave directly to boil the water off?

3.5 % yield almost three times the usual yields. This might have to do with the initial citric acid boil. The citric acid will saturate the acetone and can crash out of solution along with the mescaline. Does you final product taste a bit acidic?

Converting your fumarate to HCl by dissolving your end product in equal amount of 10% HCl and cleaning it with acetone could get rid off potential excess citric acid. The citric acid will dissolve and the HCl won't.

I think that leaving the citric acid boil step out will result in a more pure lower yielding product.

 
AcaciaConfusedYah
#26 Posted : 1/12/2016 4:01:57 AM

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Quote:
I don't have a microwave ,but nice to see this NP free mescaline tek.

Thanks Smile

Quote:
Why are you doing the acidic boil? Usually this is done either prior to defat to make sure al alkaloids are in salt form or added to water to let the alkaloids migrate from the tissue to the water in case of a tea based extraction. In your TEK immediately after the acidic addition, you basify and dry. I think the acid boil could be left out with equal results. Did you try this?
I have not tried straight to base with this method. I bet it would work fine. I like the idea of properly lysing the cells, and removing the alkaloids from their original position inside the cells and into the aqueous mix. In my logic, this would allow for more alks to be removed from the mix faster than a non lysed mix. This assists with speed of pulls. Since Calcium Hydroxide is partially soluble in water, it is best to do pulls fast.

This is because water and acetone are miscible. Acetone evaps quickly, which naturally cools the mix. As the acetone mix cools, it acts as a condenser for atmospheric water. So, the shorter exposure of Calcium/acetone/atmospheric water, the better.


Quote:
Also why did you dry the cactus first and than immediately rehydrate it in the next step? Why not putting it in the blender fresh and then in the microwave directly to boil the water off?
To get dry weight of cactus, per request of another Nexus member. Many people work with dry cactus. It could easily be blended and extracted. And that has been done by some of the people who have tried it, if i properly recall.
Quote:

3.5 % yield almost three times the usual yields. This might have to do with the initial citric acid boil. The citric acid will saturate the acetone and can crash out of solution along with the mescaline. Does you final product taste a bit acidic?

Hmm.. not sure that the citric could have done too much. It was strongly based before doing any acetone pulls.

I would imagine that the contamination came from over titration of FASA in the inital attempts.

There was some acid contamination in the fumaric attempts. Which is primarily why I have edited the original tek to advocate sulfuric as the preferred acid.


Quote:
Converting your fumarate to HCl by dissolving your end product in equal amount of 10% HCl and cleaning it with acetone could get rid off potential excess citric acid. The citric acid will dissolve and the HCl won't.

I think that leaving the citric acid boil step out will result in a more pure lower yielding product.


Interesting! If you decide to give it a try, please inform us on this thread, and post any updates!

I, unfortunately, have no more cactus to extract until next harvest season. Smile
Have a great day!
 
Tryptallmine
#27 Posted : 1/15/2016 1:48:49 AM

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Hey ACY,

I gave this tek a shot today and I'm not sure it's gone so well. Nuked and added CaOH and MgSO4 and it was nice and crumbly dry as depicted.
Made the FASA solution and performed my first pull only to have it rehydrate back to an aqueous solution? I've had to put it back into a 500ml flask to try to get it to separate aqueous layers.

Thoughts? I'll throw up a picture.
 
Mindlusion
#28 Posted : 1/15/2016 4:09:57 AM

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Curious, what concentrations of sulfuric acid are you guys using to saturate your acetone?
I mention it because there is a big difference between concentrated and not concentrated, and there has been no mention of concentration so far. You don't want acetone boiling in your face. Not to mention enough of it will actually dehydrate the acetone itself.. I am assuming nothing more than 3 or 4 drops? ( I am also imagining about 150mls of acetone, I should have mentioned that)
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Tryptallmine
#29 Posted : 1/15/2016 6:47:49 AM

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Tryptallmine wrote:
Hey ACY,

I gave this tek a shot today and I'm not sure it's gone so well. Nuked and added CaOH and MgSO4 and it was nice and crumbly dry as depicted.
Made the FASA solution and performed my first pull only to have it rehydrate back to an aqueous solution? I've had to put it back into a 500ml flask to try to get it to separate aqueous layers.

Thoughts? I'll throw up a picture.


Well there seems to be a lot of precipitation from the FASA that i've left to evaporate. Tastes like mescaline? It's not acidic so I doubt its a contamination of citric or fumaric acid.
I'll dissolve it in DI once its completely evaporated. Probably only about 300-500mg.
 
AcaciaConfusedYah
#30 Posted : 1/15/2016 10:58:16 PM

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Mindlusion wrote:
Curious, what concentrations of sulfuric acid are you guys using to saturate your acetone?
I mention it because there is a big difference between concentrated and not concentrated, and there has been no mention of concentration so far. You don't want acetone boiling in your face. Not to mention enough of it will actually dehydrate the acetone itself.. I am assuming nothing more than 3 or 4 drops? ( I am also imagining about 150mls of acetone, I should have mentioned that)



This is NON Concentrated Sulfuric acid used as "pH down" for ponds or aquariums. And yes, very small amounts. For 150ml acetone, maybe 6-7 drops should do. You should notice it begin to precipitate in the acetone, slightly.

Thank you for bringing this to my attention. I have adjusted the original post to include the concentration info. Smile


Quote:
Tryptallmine wrote:
Hey ACY,

I gave this tek a shot today and I'm not sure it's gone so well. Nuked and added CaOH and MgSO4 and it was nice and crumbly dry as depicted.
Made the FASA solution and performed my first pull only to have it rehydrate back to an aqueous solution? I've had to put it back into a 500ml flask to try to get it to separate aqueous layers.

Thoughts? I'll throw up a picture.


Well there seems to be a lot of precipitation from the FASA that i've left to evaporate. Tastes like mescaline? It's not acidic so I doubt its a contamination of citric or fumaric acid.
I'll dissolve it in DI once its completely evaporated. Probably only about 300-500mg.


I found that the mix did not redissolve when I do the pulls. It quickly settled in container and was no issue to pour off the acetone. I also used the lid of the container to create a semi-seal and restrain the mix from being poured off with the acetone, except for some of the smaller sediment.

I'd love to see some pictures of your product so we have additional references. Does it have a sour or a bitter taste to it? Did you do any wash steps to clean it up?






I am going to be doing the tek in the next few days with a piece of Peruvian torch due to an unfortunate/unexpected loss. I will be skipping the steps of drying the cactus, it will be going straight from the freezer into the blender, and then into the microwave for partial dehydration. I'll let you all know how it goes. I will be using the non concentrated Sulfuric acid to perform a SASA precipitation.
Have a great day!
 
Tryptallmine
#31 Posted : 1/16/2016 1:30:41 AM

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AcaciaConfusedYah wrote:
Mindlusion wrote:
Curious, what concentrations of sulfuric acid are you guys using to saturate your acetone?
I mention it because there is a big difference between concentrated and not concentrated, and there has been no mention of concentration so far. You don't want acetone boiling in your face. Not to mention enough of it will actually dehydrate the acetone itself.. I am assuming nothing more than 3 or 4 drops? ( I am also imagining about 150mls of acetone, I should have mentioned that)



This is NON Concentrated Sulfuric acid used as "pH down" for ponds or aquariums. And yes, very small amounts. For 150ml acetone, maybe 6-7 drops should do. You should notice it begin to precipitate in the acetone, slightly.

Thank you for bringing this to my attention. I have adjusted the original post to include the concentration info. Smile


Quote:
Tryptallmine wrote:
Hey ACY,

I gave this tek a shot today and I'm not sure it's gone so well. Nuked and added CaOH and MgSO4 and it was nice and crumbly dry as depicted.
Made the FASA solution and performed my first pull only to have it rehydrate back to an aqueous solution? I've had to put it back into a 500ml flask to try to get it to separate aqueous layers.

Thoughts? I'll throw up a picture.


Well there seems to be a lot of precipitation from the FASA that i've left to evaporate. Tastes like mescaline? It's not acidic so I doubt its a contamination of citric or fumaric acid.
I'll dissolve it in DI once its completely evaporated. Probably only about 300-500mg.


I found that the mix did not redissolve when I do the pulls. It quickly settled in container and was no issue to pour off the acetone. I also used the lid of the container to create a semi-seal and restrain the mix from being poured off with the acetone, except for some of the smaller sediment.

I'd love to see some pictures of your product so we have additional references. Does it have a sour or a bitter taste to it? Did you do any wash steps to clean it up?






I am going to be doing the tek in the next few days with a piece of Peruvian torch due to an unfortunate/unexpected loss. I will be skipping the steps of drying the cactus, it will be going straight from the freezer into the blender, and then into the microwave for partial dehydration. I'll let you all know how it goes. I will be using the non concentrated Sulfuric acid to perform a SASA precipitation.


So here is a couple of pics. My starting material was powdered so finely you could have railed it happily.
You have the picture of the mix that I had to transfer into the flask as it became exactly like a normal A/B aqueous extraction when 200ml of FASA was added. It bubbled quite a bit and reacted before settling.

The tray is approx 400ml (more like 100 now) of the first 2 pulls I did that is evaporating under a fan. It has quite a lot of powdery granules in it. It smells like cactus product however the acetone has completely lost its keytone aroma. Wondering whether I should keep evaporating the whole tray or filter it and titrate again with more FASA.

Having tasted some of the paste and tasted some lime, I suspect its calcium hydroxide contaminated mescaline if anything at all. There looks like two shades of granules starting to precipitate out - but it smells like cactus tea quite strongly.

One of the issues I faced was getting the fumaric acid to even dissolve in cold anhydrous acetone. I measured out 1.2g for 200ml and almost none of it dissolved in cold acetone or room temp acetone. Kind of odd.
Tryptallmine attached the following image(s):
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precip1.JPG (98kb) downloaded 497 time(s).
precip2.JPG (104kb) downloaded 503 time(s).
 
AcaciaConfusedYah
#32 Posted : 1/16/2016 12:12:14 PM

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Eeeek. Yeah, it seems like you did make some pretty big errors there.

Did you use dehydrated magnesium sulfate at all? I didn't see any mention of it. The tek is like baking a cake. It will not work if it is not done right.

Probably best for you to take the route you are more comfortable with. The mescaline is still recoverable.
Have a great day!
 
Tryptallmine
#33 Posted : 1/16/2016 11:13:13 PM

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AcaciaConfusedYah wrote:
Eeeek. Yeah, it seems like you did make some pretty big errors there.

Did you use dehydrated magnesium sulfate at all? I didn't see any mention of it. The tek is like baking a cake. It will not work if it is not done right.

Probably best for you to take the route you are more comfortable with. The mescaline is still recoverable.


Sure did, dehydrated in the microwave, mixed half in with the acetone and half into the mix with calcium carbonate.
It's all good, I'll be able to recover it. I'll kill all my posts to clean up the thread.

*********

I did some tests, the acetone never dried from the MgS04 hence it all merged into one solution. The goo that was left in the dish dissolved in a weak HCl solution and not in acetone or methyl ethyl keytone. However with the amount of MgS04 and CaOH I used initially to dry it up that was caking on the inside of my flask, I opted to flush it all down the sink. All a bit of fun!


 
AcaciaConfusedYah
#34 Posted : 1/17/2016 4:01:34 AM

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It's ok to leave the posts - unless you would like to pull them.

I know that some people will have issues with this tek, or any tek, from time to time. I'm glad that you tried it, and sorry that it was not more rewarding for you.

It's probably a good thing that people post any issues or problems. That allows me to consider how I'd like to adjust the tek to make it better. It's still a work in progress.

It's actually changed a lot since it was first tried, and changed a lot since being published. For example, deciding that the sulfuric acid might be the best choice over fumaric or citric. However, when I published the tek, I had only tried citric and fumaric. And when I first attempted it, I only used citric - no fumaric or sulfuric.

It may be making a huge change depending how my next extraction goes. May be cutting out the pre-dehydration step all together. Freeze, partial thaw, blend, microwave assisted acid cook/dehydration.

So the tek grows. Maybe I need to revisit all the wording, and see if I can make it more clear in certain areas.


Have a great day!
 
mateo
#35 Posted : 4/20/2016 6:07:01 PM

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I'm on the last stage of the process. I pulled with acetone, added sulphuric acid, and placed in the freezer for 6 hours. Did not see much precipitation, I figured some lime dust slipped through my filter, so I decided to add more sulphuric acid and place back into the freezer over night. After still not seeing much I decided to evaporate it. This is a picture of what I got. What would be the next best step at this point?
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ManicMongrel
#36 Posted : 4/23/2016 11:02:11 AM
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@AcaciaConfusedYah: Thanks again for a very practical tek. This is definitively a viable approach when working with T. peruvianus and T. macrogonus, which does not combine all that well with xylene and toluene based teks. Also acetone have the benefit of low toxicity and super convenient volatility.

I have recently tried this with phosphoric acid and can confirm that an alkaloid salt quickly phases out of the acetone and forms tiny crystals. I think I will prefer phosphoric acid over fumaric acid and sulfuric acid for now, since it has better solubility in acetone.

I'm working with T. peruvianus powder atm, and have tried pretty similar approach to this tek with bioethanol as a first step to get crude extract. First I soaked the dry cactus powder in the ethanol, then added a tiny bit of water so that the powder swelled a little, then added a bit of sodium hydroxide and let it soak for a couple of weeks before separating and drying the solvent. The dry resin was then soaked in acetone, phosphoric acid was then gradually added to separate the alkalic fracton from the brown acetone. The next step is to recycle the acetone and use it to pull more alkaloids from the resin (residual acid was removed from the acetone with sodium cabonate first).

I haven't tested these phosphate salts to confirm that they contain mescaline yet, but I'm optimistic.

(Materials: Phosphoric acid 75%, approved for cleaning of equipment in food production. Bioethanol 90–98% ethanol, 2-10% heavy alkohols.)

@Mateo: you can dry the resin in a vacuum container for a few days, then try to wash with acetone and sepparate with a coffee filter. If the product is too fine-grained to be separated with a filter, you could add a tiny bit of water to the resin, then dry it up again in the vacuum box to get larger crystals, which won't pass though the filter.
 
skoobysnax
#37 Posted : 8/25/2016 5:45:29 PM

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I am finishing up my first try. The result looks cleaner than I expected. After I filtered the acetone I didn't see any residue floating around when I salted it with the PH Down sulfuric acid. I did see alks crashing when i titrated the acid, not thick like salting dmt fumarate but cloudy nonetheless.

I started with a larger amount than the demo tek and ended up with a large amount to base and dry so I lost a whole lot of solvent. Used a t shirt to squeeze out all I could, let that tone settle and filtered through a glass wine bottle funnel stuffed with cotton to yield a sediment free solvent. the yield was about 380mg from about 50G of cacti (1/2 san pedro 1/2 Peruvianus) and the solvent is still evaporating.

I am curious though if some lime or magnesium sulfate got through and if so how do I clean that since a cold acetone cleaning probably wont dissolve them? maybe I am overthinking a problem that doesn't exist...

I am in no rush so I can wait until I hear some input.
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skoobysnax
#38 Posted : 8/25/2016 5:46:54 PM

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P.S. smells like cactus...
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Entheogenerator
#39 Posted : 10/19/2016 12:54:49 AM

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I'm also currently working on this tek, and I was wondering if anyone could advise me as to how one would go about precipitating the alks out of the acetone solution using concentrated sulphuric acid? Would you simply use less, adding it dropwise? Or would diluting it with distilled H2O be a better solution? I don't want to proceed without advice as someone mentioned earlier in the thread the possibility of the acetone boiling violently, I'm assuming if too much were used. Can anyone shed some light on this issue? Thanks Thumbs up
 
Tengukashi
#40 Posted : 2/15/2017 11:22:28 PM

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I see a way this tek could be altered to allow for easy hydrochloride extraction: replace the acetone with Isopropyl Alcohol. The pulls from the cacti would be evaporated (reclaimed through rotovap/distillation if possible), then fresh, cold, dry as possible IPA added. As little as possible to encourage precipitation. Then dry HCL added, or hcl gas bubbled through the IPA. Crystals should precipitate readily.

I attempted the original tek a few weeks ago, and sadly I don't think any product precipitated. I saw some crystals precipitate from the Acetone, but they redissolved when put in the freezer. I used battery electrolyte, since most aquarium stuff is far less concentrated. Might've made the solution too polar and the sulfate easily dissolved, or the cactus wasn't dry enough, since I used a freeze-thaw cycle instead of the microwave...should've microwaved it.
 
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