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Mescaline HCl purification Options
 
pete666
#1 Posted : 6/11/2018 1:57:12 PM

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If pure mescaline is what you are after, here is technique I use. It is working and tested procedure for peruvian torch dried green tissue. But I would bet it works for other sources as well. It uses techniques used by others on DMT Nexus or elsewhere. It just pushes the cleanup a bit further and is quite detailed.

The reasons for pure mescaline are numerous. Off-white or tan-white powder still contains other chemicals. They may be/are psychoactive, but for many, they just make mescaline experience worse. Some people are using MAOI (moclobemide, harmala, ..) and purity here is a must. Another reason might be just aesthetical. Not a big deal when ingesting orally, but for rectal ROA the powder has to be dissolved in water and even almost white powder can turn into dark brown when in contact with water. Injecting this is much less desirable than pure white liquid. And of course, any impurity affects dosage. Last but not least, mescaline is a tool. And purity of tool can influence the result.

Salting phase of mescaline extraction calls for pH 7 for the most pure results. Unfortunately this pH is not low enough for all mescaline to transfer from np into water. We should target for pH 5,5. But with lower pH, more impurities find the way into water too. But even with pH 7, result likely won't be pure mescaline. I prefer targeting pH 5,5 with proper purification later.

This procedure contains two other techniques : mescaline wash by acetone/IPA/MEK and activated charcoal purification. Unfortunately re-x of mescaline HCl (unlike sulphate) is quite tricky and because of that it is not used. I wish we had something like heptane for dmt re-x here!
After wash with dry/freezing solvent mix, the result is off-white or white mescaline. Nice, but there are still impurities (although invisible) within the molecular latice. I would estimate about 20% of impurities is still there. We need to dissolve it in water and remove while liquid - we use activated charcoal. Expect about 8% loss due to the activated charcoal purification

I strongly suggest using proper glassware, lab-grade chemicals and filters if possible.

*************************
EDIT : endlessness was kind to arrange analysis of products of this procedure (thanks a lot), here are the results (source - dried chips from reputable Peru source, STB + cleanup) ...

1- Raw Mescaline (result of STB + back-salting) - 77% mescaline
2- Washed Mescaline - 85% mescaline
3- Washed remains - 26% mescaline
4- Washed + activated charcoal - 94% mescaline
5- Washed + activated charcoal + re-x - 95% mescaline

*************************

The procedure:

After salting and evaporation, we get result of various quality on the dish. How to purify it?

1. Scrape the result and break it AS MUCH AS POSSIBLE with mortar and pestle. It has to be the finest powder. The finer, the less activated charcoal will be necessary later
2. Put it into oven at 80C for few hours. Mescaline HCl is very heat-stable, it can be there for very long time without any problem. Break by pestle every 15 minutes as it is drying
3. Optional but highly suggested - put it into small paper envelope and place the envelope within small air-tight container with bottom full of dry MgSO4 (dried epsom salt) for few days(1 day is ok, 3 days are better). We want to get rid of any water, as it causes lower yields
4. Prepare mix of dry! acetone, dry! IPA and dry! MEK (ratio 1:1:1). Mix properly and put it into freezer for a day. MEK is not necessary, but tone and IPA yes. I use all. Any water in this solution leads to lower yields
5. Optional - prepare your environment. We need low temperature and low humidity of the air. Freezing solvent mix can (and will) absorb water from the air, so we want to avoid it as much as possible. Air-cond running on max for half day is a way how to achieve it.
6. Use round bottom evaporating dish with spout of proper size (mescaline + solvent should be 1/3 - 1/2 of the volume of the dish). Put there dry mescaline powder.
7. Pour enough mix from step 4 to cover the mescaline. The volume is not very important, it may be more. Use pestle to mix it for about a minute or two.
9. Tilt the dish to one side and leave for few minutes to settle. Then lean slowly to the opposite side, so solvent moves but settled mescaline doesn't. Use glass pipette with rubber bulb or eye dropper to remove the solvent. Remove as much solvent as possible. Pour removed solvent through funnel with proper paper filter (grade 3 - particle size 6µm) or enough cotton.
10. Repeat steps 7-10 until solvent is almost clear. Usually about 3-5 washes are enough
11. Pour as much solvent as possible out of the dish through the filter
(Solvent can be evaporated to yield oily dark mix of other alkaloids. Active at about 150mg for peruvian torch)
12. Dry the dish with mescaline - put the dish in a warm/hot bath (60-80C) for half an hour and then put the dish and the funnel/filter paper into an oven at 80C for an hour
13. Dissolve mescaline from dish and filter/cotton in distilled water and put into beaker. I use about 10ml of water for each gram of mescaline.
14. Add activated charcoal powder - I usually use 5% of the weight of the mescaline. Be careful, you don't want to have activated charcoal anywhere else than in it's container, on the spoon, in the beaker or later in the filter. It is almost impossible to get it out of most surfaces! However, it is quite easy to work with when done with caution. If you don't use powder, you have to adjust the amount. But be careful, too much charcoal means bigger loss. It is much better to add the charcoal incrementally, mix few minutes, let settle and check the color than to use too much at once and lose the precious medicine
15. Put into hot/boiling bath (90-100C), let get hot and mix for about 15 minutes
16. Pour everything through the funnel with paper filter(grade 1 - particle size 11µm) or cotton
17. When the filter is empty, pour another pure hot water through it to get last traces of mescaline. Discard filter with charcoal
18. Evaporate water
19. Enjoy with humbleness

Comments:

Always bear in mind - Water is our enemy in the washing process. Everything (air, glass, tools, hands, solvents, source mescaline material) has to be without any water. Water means losses.

Step 4 : The drying process is the same for all 3 solvents

Step 7 : Keep the solvent in the freezer as much as possible

Step 9 : We don't mind warmer solvent while waiting for settling down, we are not mixing it, so it is not dissolving our precious medicine.
Use filter rather than cotton, you may lose the goodies

Step 10 : No problem with doing more washes. If done properly, the loss is minimal

Step 12 : Many people can stop here. The product is almost white. The impurities are hidden in the molecular latice and almost invisible.

Step 14 : You can use any activated charcoal, it doesn't have to be powderized

Step 15 : If you remove it from heat source, so it is not boiling and wait a minute or two, it will clear up. You can see whether purity is as desired. If not, mix or add a bit more of charcoal

Step 16 : If unsure, try it first just with water and charcoal so you get practice
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Orion
#2 Posted : 6/11/2018 6:06:56 PM

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Pretty good. I like the idea of using mek, iso and acetone to cover all bases.

I always aim for about PH 6 for salting, but the molecule itself pushes the PH back up as it migrates. You have to accept that there has to be a balance between salting strength and purity unless you have time to do a lot of salting and evaporating.
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pete666
#3 Posted : 6/11/2018 7:20:11 PM

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Yes, it pushes but only while there is anything to push, once all is salted, it goes steeply down
I am accepting some HCl in the salting result. Everything goes twice through evaporation/oven heating later, so all HCl is left behind (evaporated). Whole evaporation is always done at air temperature over few days, only final step is in an oven at 80C
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antichode
#4 Posted : 6/17/2018 9:32:12 AM

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You know, if you use sulfuric acid your mescaline will crystallise directly in the salting water (once reduced) and this will leave all impurities behind in the water. Tip the water out then a quick rinse with acetone to remove the crystals before drying. The water still contains mescaline so you can add acetone untill everything crashes out but that will likely crash impurities as well. The initial crystals however. Super clean!
 
pete666
#5 Posted : 6/17/2018 10:01:03 AM

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Yes, I am aware of that. Unfortunately the solubility of mescaline sulfate is poor and I need to dissolve quite a lot in one or two milliliters of water, because of rectal roa.
I had the salting by sulfuric acid for purification and then basification and salting with HCl as one of possible ways. But it was not selected, due to probability of lower yields and existence of better method.
I was always curious, when titrating with sulfuric acid, one has to target pH 7, so excessive acid is avoid in the result, right? But with this pH there is still mescaline freebase (mescaline is not protonated). Is it sacrificed? Or is it extracted somehow?
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antichode
#6 Posted : 6/18/2018 5:39:29 AM

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pete666 wrote:
I was always curious, when titrating with sulfuric acid, one has to target pH 7, so excessive acid is avoid in the result, right? But with this pH there is still mescaline freebase (mescaline is not protonated). Is it sacrified? Or is it extracted somehow?


Im no chemist but from experience, once you hit ph 7 and its stable, very very little acid is needed to dip the ph well below 5. This indicates to me that very little freebase is left. The amount that is sacrificed is worth the purity if you ask me! Emulsions also seem to become worse below PH 7 for some reason.
 
pete666
#7 Posted : 6/18/2018 6:50:44 AM

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antichode wrote:

Im no chemist but from experience, once you hit ph 7 and its stable, very very little acid is needed to dip the ph well below 5. This indicates to me that very little freebase is left.


Yes, my experience with HCl salting/titration is the same. There can't be much

antichode wrote:

Emulsions also seem to become worse below PH 7 for some reason.


I had emulsions when salting only at room temperature. I am always warming it up to 60C. Separation is perfect after mad shaking within seconds.
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DrSeltsam
#8 Posted : 6/18/2018 9:57:07 AM

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pete666, very nice research you have done! Thanks a lot for posing this! I opened a very similar thread (Purification of Mescaline HCl, perhaps we can merge them to collect the knowledge a bit better?

I can not support your sentence "Unfortunately re-x of mescaline HCl (unlike sulphate) is quite tricky and because of that it is not used." I think it is very easy to do: just use dry IPA and you are good to go. The crystals I got were slightly tanned but I don't think this is a problem. Other people pointed out going to FASA is also a very good route to clear up the HCl salt.
 
pete666
#9 Posted : 6/18/2018 1:38:20 PM

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DrSelstam, I have read your post before and all other posts about mescaline cleanup. I liked the (analytical) way you did the tests, although the result was a bit confusing. But simply this is how it is. Those procedures have many variables, so the results are variable too.
In my experience a small detail, often overlooked, may have huge impact and later it is very difficult to say what caused what.
I know about acetone, MEK or IPA re-x. I have read all available info on the web. My impression (maybe wrong) is that those can't be used for re-x in reasonable amounts, when anhydrous. The solubility of mescaline hcl is simply too low. There has to be some water in it, so in fact it is two-solvent re-x. People have different quality of such solvents, with different contents of water. Their humidity is unknown too, and their technique as well, so in fact it is very difficult to predict final content of water in the solution and final loss.
I had very tough time trying to dissolve mescaline hcl in those solvents. But I had them anhydrous, lab-grade, of the best available purity. It may be possible to define water/solvent ratios, to maximize purity and minimize losses, but it is not as simple and requires some trial/fail.
Activated charcoal compared to re-x is pretty straightforward. It is done in water, humidity doesn't play any role, amount of water neither. It can be added in small steps until the solution is clear, so minimum necessary is used and it is removing exactly what we want, so losses are minimal when done properly. Simple and predictable.
However, everyone has different requirements, thoughts, materials available. So everyone can use different technique here.

I don't have an idea how to merge those threads that it would make sense. Anyway, link to your topic is here, so anyone interested may go there and decide which way to go.
It would be nice if we could edit the wiki and add the techniques there. But as far as I know, this is not possible atm.
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DrSeltsam
#10 Posted : 8/15/2018 3:49:29 PM

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Hi pete666,

Sorry for the late reply. Please don't take this personally - it was me having too many other things in my life lately.

Thanks for the compliment that my tests are very analytical Smile I find your posts very well written as well - probably even better for non-experienced people compared to my posts. So please don't take the following points personal.

1.) I would encourage you to send the results of your purification to EnergyControl (details in this thread). Eventually the proof is in the numbers Pleased

2.) Regarding your comments on the recrystallisation. You are right in a sense that my posts are not super reproducible but that is just the way it is with these kind of things in chemistry. Normally, the whole process that I describe on several pages is summarised as "The substance was recrstallized from IPA" in the literature (look at these examples. If the author was in a good mood, he might add minor details but not more. Notice that no-one ever give guidance how long it takes to dissolve the substance when doing this. Mescaline in IPA took about 15 minutes for me but hours are not unheard of).

Perhaps you are right and what you did (and I fully appreciate the fact that you did it and took the time to write it down) is better suited for a formal tek. From my point of view this is s.th. still missing and would be cool to put on the wiki.

Keep up the good work!
 
pete666
#11 Posted : 8/15/2018 8:51:20 PM

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Hey DrSeltsam,

I am not a member of any forums except this one. I don't have the urge to share information except information regarding entheogens. This has very deep value for me and I owe them a lot. The same with Nexus.

I am not a chemist, I just did search and study (mostly here) and followed the voice in my head/heart. It showed me the path to pure product, both for dmt and mescaline extractions. And I am honestly thankful! My entries here are nothing new, maybe just some small tweaks were made to make it even better.

It's not likely to be personal, because we are both trying to reach the same goal. I recognize and appreciate such endeavours.

I would really like to have the result of the purificaiton tested. Unfortunately the first condition is not met. My all extracts are from commercial product.
I have a lot of cactuses growing, but they will be ready for harvest next year in October, so then I can proceed with it.

Regarding re-x, I am sure I will try it sometimes, once I can afford it. But just now the entry material costs a lot of money and it is very precious for me. My motivation to try anything else is very low, when I have perfectly working method. But once I have my own ripe cactus, I will likely go through your topic and try it again.

Take care my friend
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pete666
#12 Posted : 8/16/2018 10:31:57 PM

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endlessness offered the possibility of testing. I will prepare the samples soon and we will proceed with the test.
Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
pete666
#13 Posted : 11/14/2019 3:40:55 PM

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Here are the results (source - dried chips from reputable Peru source, STB + cleanup) ...

1- Raw Mescaline (result of STB + back-salting) - 77% mescaline
2- Washed Mescaline - 85% mescaline
3- Washed remains - 26% mescaline
4- Washed + activated charcoal - 94% mescaline
5- Washed + activated charcoal + re-x - 95% mescaline

Thanks a lot endlessness!
Acceptance of the fact that our reality is not real doesn't in fact mean it is not real. It just leads to better understanding what real means.
 
leratiomyces
#14 Posted : 11/14/2019 7:29:48 PM
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Nice work!
What other compounds are in the raw mescaline? Ie. the other 23 percent?
 
Tony6Strings
#15 Posted : 11/14/2019 8:13:46 PM

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Very cool, I admire your devotion.
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