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Crystal Clear Mescaline HCL -- easy as pie


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#41 TVCasualty

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Posted 05 November 2007 - 09:31 AM

Sweet, great thread! This is one I'll have to try someday.

Have you looked into using a molecular sieve for drying solvents? I believe 3 angstrom zeolite would be the right size for water. Zeolite is used for making E85 fuel, since there cannot be any water in the alcohol for that application (gives you 100% ethanol, and would likely work with xylene and acetone as well, though I haven't tried anything but alcohol).

C'mon down to Dessicant City for your anhydrous needs... http://www.agmcontai...lecular_sieve_1

#42 Myco-Iggy

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Posted 05 November 2007 - 11:07 AM

All your contributions will be put to use,
Thanks again and wonderful input!

Ig

#43 tregar

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Posted 05 November 2007 - 05:53 PM

Thanks TVCasualty, appreciate the dessicant & sleeve info, that would most likely work, thanks again! I've wondered where a person could find them.

Nice sulphate crystals you had there in the photo earlier, nice work myco-Iggy. I'd be very proud of those.

Good luck everyone, I'll be around, trying 250mg soon this week.

#44 tregar

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Posted 07 November 2007 - 11:36 AM

This may sound weird, but the alkaloids extracted directly with water gave me an experience comparable to the whole syrup. This was from the 4rth pull, collected directly with water.

I'm gonna do white's re-crystallization to get some transparent-like crystals eventually, I want to get it as super-clean as possible.

I have not yet taken the alkaloids that ended "on top" the filter yet, but soon.

Strange images and lifeforms were seen with closed eyes towards the tail end of the experience. I saw a fully formed alien being materialize from the dark patterns in front of my closed eyes. Higher doses will brighten up the patterns & images and bring out more of them. I couldn't believe how powerful the experience was, yet still totally relaxing. After the 2 hour comeup, we laughed hysterically for hours and hours at everything on tv (we watched the movie 'waiting' too) and music sounded really far out...220mg felt comparable to 1.5 hits of strong acid, tripped very nicely. Whoever saids mescaline doesn't make you laugh is wrong, this stuff had us laughing un-controllably for hours upon hours...just like the laughfest acid gives you, all the while slight visual stuff going on around us. Experience lasted from 7pm to 2am, when we went to sleep easily.

No nausea, but some burping and gas were felt by both of us during the 1st 2 hours, this was most assuredly due to the fact that I need to clean my product more (has large trace amounts of yellow in the 4rth pull of the product with water), a warm/hot acetone wash or using white's re-crystallization should be the ticket, I will get started on this eventually. It is quite significant that my girlfriend experienced no nausea at all...even at this dose, whereas in the past she has gotten nausea and stomach "ickyness" from product that was a/b collected (typical salting) then acetone washed. Should I get the product even cleaner, we will both be extremely happy, no doubt to just eliminate the gas and belching sensations for the 1st 2 hours. The water does pick up some "crap" from the xylene when I collected directly with water still from the 4rth pull at least, yellow looking...this must have been what caused the "belching" early on.

Extremely enjoyable experience, pleasant afterglow today.

As an alternative to using water to collect the alkaloids from the sep funnel, another way of collecting the alkaloids, would be to just let them all fall to the bottom of the sep funnel after 1/2 hour, then drain them out into a little "puddle" it will have some xylene in it, but it will evaporate off...then just clean the crap out of the puddle with a xylene rinse perhaps, then wash and rinse it several times with acetone as Avalo describes, then chop it up and add it to boiling hot water to drive off any solvent fumes, proceed with Avalo's cleaning procedure below...I will do that next time. This will also give you the full alkaloid effect by letting all the alkaloids fall to the bottom of the sep funnel, then drain them off, will be "bright yellow" in color. Most of the xylene will then evaporate off, proceed with acetone cleaning, then wash and rinse with more acetone and use boiling hot water to drive off fumes, proceed with re-crystallization. See this post:

Avalo said:

Instead of just using water to extract the mescaline.hcl from the gassed xylene, I'd suggest filtering it using a bit more clean up, then an acetone/water recrystallisation.

Post Gassing Clean-up
Filter the mescaline.hcl from the gassed xylene. (or let them collect at the bottom of your sep funnel, then drain off the mescaline puddle at the bottom: editor's note: it will be a bright yellow puddle: tregar)
Then wash the powder with clean xylene. This flushes through any brown cactus crap that was also in the xylene.
Now disconnect the vacuum hose to break the vacuum. Then reattach it, but leave the vacuum turned off. This creates a sealed volume of air, so when you pour liquid on top of the filter paper, the trapped air will tend to keep it there instead of allowing it to drain through.
Now using a wash bottle, wash the powder with acetone until it's completely covered, and let it sit for a couple of minutes. Then turn the vacuum on, and filter through the acetone. Now rinse the powder with more acetone as it's being sucked through. This soaking and washing will remove the vast majority of the xylene.
Cover the filter funnel with a large oversized piece of filter paper, and suck air through the funnel for a couple of minutes, this will help dry the powder and protect it from dust.
Now remove the filter funnel and allow the powder to completely dry.
Once dry, the power will flake off the filter paper, so you won't get mushy paper fibres in with your product.

Acetone/Water Recrystallisation
Place the mescaline.hcl powder in small 50 mL flask.
Use hot distilled water to soak the filter paper, and wash the filter funnel.
Add this to the flask, and then add a small boiling chip.
Using a flame or oil bath, boil the water down until it starts to get a sheen on the surface.
The boiling water will drive off any residual solvent vapours, and you boil it until the mescaline gets concentrated.
Then remove it from the heat, and let it cool down a bit.
If crystals start forming immediately, then you've boiled off too much water. So add a bit more water then re-heat it and boil it down again.
Once the solution is concentrated and warm but not hot, then add an equal volume of acetone. Crystals should start forming immediately.
If the crystals don't form when you add the acetone, then there was too much water in there, so boil it down again. The acetone will all boil off first, then boil off a bit more water before letting it cool and re-adding some more acetone.

Once you add the acetone and the crystals start forming, then reheat it, and drip in a single drop of water at a time, until all the crystals dissolve in the hot acetone/water solution.
Then remove the boiling chip and let the solution slowly cool down to room temperature, then place it in the fridge.
Filter the pure crystals out.
You can also recover the mescaline traces and impurities by evaporating off the waste liquid on a Pyrex dish.

The recrystallisation is a bit of mucking about, and I hear it takes practice to master, I've only read about this at the moment. But the trick is to get the crystals to grow out of the solution as it cools. If you crash the crystals out too soon, then they form small crystals that grow very fast and trap impurities inside the crystal matrix.

The other thing you can do to remove solvent residue is put your powder or crystals in a short test tube and place them inside a filter flask. Put a solid bung in the top and then turn the vacuum on. The reduced pressure makes the solvents evaporate off much more quickly.



#45 tregar

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Posted 07 November 2007 - 07:44 PM

More on Re-crystallization to obtain crystal clear mescaline hcl (for the advanced hobbyist), also see the above thread.

white:

With foaf's tek shouldn't we be knowing how soluble these solvents are in water? that would be the true issue for final purity as they would be carried with the water/salt to the drying tray. In this regard I always take my washed product and redisolve it in boiling ETOH 95% and boil till reduced by half. I am quite sure to have boiled out any residual toxic solvents A final filter thru cotton with hot ETOH washes and the hot liquor is left to slowly Xtalize while evaporating leaving largish opalescent beige plates in the drying vessel MP 177-179.
with a very slight honey aroma.


Persona:

What I would personally do:

Dry your xylene. Your work shows that this is necessary in the case of extractions. To do this, washing the xylene with a concentrated salt solution would be good to get any ionic impurities out, followed by a more thorough drying with CaCl2 or MgSO4. Be sure to very thoroughly decant or filter well your xylene if you use CaCl2 as your drying agent.

Next step, gas. Once everything is gassed, filter your xylene and crystals with a #103. The collected crystals are then washed with acetone (which in answer to your earlier question, would pick up just about any non-ionic impurities, many of which are nasty cactus alkaloids ((IMHO))). The crystals on the filter are then transferred to a new filter, washed once more, once with acetone, and if you are shooting for purity, cold isopropyl alcohol (this will wash out any impurities and remove any water present in the acetone).

You can then evaporate your solvents to recover whatever your gassing/washing dissolved, and recrystallize if you want.

---

As far as using ethanol to wash, this is for all intents and purposes a regular recrystallization as I understand it. You are basically doing the same steps mentioned, except by using the cotton filter and hot ethanol, you are dissolving the mescaline, allowing it to filter through cotton, which takes out any non-ethanol soluble impurities, and then recrystallizing from ethanol.

Personally, I would go with a more defined recrystallization. The easiest thing to do would be to isolate your crystals as per the method given, and recrystallize from USP grade 91% isopropanol and dH2O. Using these two would ensure purity. Put your crystals in a beaker, heat isopropanol on a water bath till a boil, cover the crystals and slowly start adding hot dH2O until they are dissolved (this whole process is done while the isopropanol/water/mescaline solution is boiling). Then continue heating and add a few drops of room temperature 91% isopropanol, until you start seeing a very very slight film or precipitation develop. Then remove your water bath from the heat, cover it with a towel (with the beaker still in it), and leave it alone and completely undisturbed, in a fairly dust free enviroment until it reaches room temperature and then some few hours on top of that. Stick the whole thing in the fridge very carefully after that, followed by into the freezer. This entire process, if you are patient and do it properly, should take around 24-36 hours. Some fairly spectacular crystals will develop, which you can then used as seed crystals for subsequent crystallizations, which save you a lot of time and also allow for extremely pure crystal formation.

The nice thing is that once you have one seed crystal, you can cut the time needed for recrystallizations quite a bit, and also can ensure purity and quality with 0 worry. Believe me, it's really worth it to try. Try and recrystallizing 1g, it will be worth it.

As far as ratios go, just figure it out experimentally. Heat your solvent and add it slowly to the crystals until they are at least covered. I would say, 5g of crystals in 25-30ml of isopropyl alcohol is reasonable. Then add water from there. It will take some time to figure out the true ideal ratios, but if you understand the concepts behind crystallization it's a cinch.

I should probably mention these now. You want to create a solution that dissolves the mescaline at boiling, but is relatively insoluble to mescaline at freezing. You want the impurities (primarily non-polar substances, or amine salts like mescaline, present in far smaller amounts) to remain soluble in solution.

If you use too much alcohol in beginning, say 100ml per 1g mescaline, you will just dissolve your crystals at all temperatures, and will need to boil down your alcohol to attain a more proper mix. So if you add too much alcohol, before adding more water, let the alcohol evaporate and then add water.

If you use too much water, you will need to evaporate the solution down a fair amount and then repeat the procedure from start basically. Avoid doing this, always add extra alcohol, not water.

If you need to adjust crystal solubility remember, adding more water dissolves more crystals, so ultimately adding 3ml of water might dissolve an entire gram... at room temperature! You need to add water slowly. If you added too much water, you would want to evaporate the water for a few minutes, then add more alcohol so that the crystals precipitate slightly upon adding the very last drop.

Once you have your idealized solution, let's say, ~90ml ~60/40 isopropanol/water @ 90C dissolves 10g of mescaline you find, at precipitates 9g at freezing (this is made up so don't actually use this to start, use the above methods)...

You start with 10g mescaline. You add 91% boiling IPA to the crystals. The beaker that the crystals are in should now be placed in the water bath, and the solvent continued to be boiled. Only a little bit dissolves. Slowly you add water in premeasured portions, say 1ml per addition, until the mescaline dissolves. So assuming you started with 60ml of 91% isopropanol, you find that after adding 27ml of dH2O dissolves all the mescaline at boiling point - specifically, you add the last drop and the last of the crystals go into solution. You heat the mixture to a vigorous boil, add another drop of isopropanol, then carefully cover and allow it to sit. After freezing you collect 9g of crystals. You evaporate your mother liquor until crystals precipitate and repeat the procedure to collect another .9g. Just remember, each subsequent collection past the first is more and more impure - so adjust the rations properly right away.

Once you collected and weighed, you can calculate the actual proportions. (That is, you of course won't know that 60/40 is the ideal mix, only after when you see that you added with much water to your solvent etc...).

Anyway, some fairly involved procedures, but really worth it. Try it on a gram or two, you won't regret it!

Remember, if you screw up, you can just evaporate your solvents and recover your product.


White:

I gave this a go using 99% iso.First attempt used too little solvent and ended up with a chunk in the freezer so redid it with 5x by volume iso and brought to heat this nearly disolved it completely. I added only one drop of water and it cleared I reduced it until it "shimmered" and cooled slowly to recover a thick layer of clear-tan xtalsfrom the alcohol these were xylene washed to remove even more "color" then boiled in etOH to clear all solvents and dried to the same color as tregars gassed product ( pics when camera gets some batteries).

MEK = methyl ethyl ketone

Results; MEK/Iso/H2O is much more efficient at collecting impurities and trapping them while releasing the alkaloid in a more pure state .Iso/water returned only 74% of the product as crystaline and held over 25% in solution after freeze precipitation it also left more color than the MEK/Iso/H2O method which generaly returns high 80 to mid ninty percent of my "crude" as off white Xtals.

80%MEK/20%ISO/ water to taste.Dropwise until it reaches shimmerosity then one or two past till just barely clear, boil until just shimmering again and slow cool.
I use 10x by volume solvent to product as fine powder.
for very clean linen white product repeat process then slow crystalize from etOH for clear needles. Pics below.

That was just for show. It can be done to perfection. For me however this is wasteful of my time and effort as the opal tan from a 'tone wash and etOH boil is as good as I need. Just wanted to show what CAN be done with practice and if it is that important to you. 'Tone ,MEK and MIBK will all work as will etOH in place of ISO but the 95% etOH I get you dropper in after10% due to the 5% H2O.
1500mg opal tan yielded 1234mg of the clear crystals pictured after two passes and an etOH boil

Questions and answer session with white:

1) Sorry for the stupid questions, but what materials are needed for this re-crystallization? Was this done outdoors or inside?

"This was inside with a wind blowing thru the room but a fume hood or outdoors is where it really belongs. I was just winging a quick sample so I just did it in the kitchen."

2) Was this done using a skillet with sand on it, and if so, how exactly is this put together? I have an erlenmeyer flask or two, is that what is used to do the heating in? Or should a measuring cup be used ?

"I like oil baths better than sand so I use a small aluminum cup and mineral oil on a lab grade hot plate(no sparks) and I have a small collection of various glass cups and labware that are pyrex."

3) Please list the materials needed if possible and how to do the heating for a novice like myself--I've never heated solvents before, and the process seems a little nerve wracking to me...please list any safety precautions, thanks!

"Use heat resistant glassware in an oil bath ( a fry daddy works good wired with a dimmer switch wired in to control temps) slowly brinng up your temp to the BP of your solvent. Ventilation should be good enough that even working over it you do not get more than a whiff of odor if any. If it smells strong it can possibly ignite so use your senses as a guide and a box fan upwind if needed. A fire extinguisher is a good idea and a box of baking soda. Good gloves help move hot glass. cool to room temp before placing in fridge,and fridge temp before freezer. Don't breathe too much solvent. treat it very carefully when hot. Expect to need a couple practice runs before you use your product. Set things up and go thru it minus the product till you are comfortable with the process and safety precautions. See why I think it's a big pain for product which is subjectively, when dosed, imperceptable from what I start with? Even doing it quick and dirty( in the house) it took most of the day to do two passes and the rexatlization from etOH. I can almost extract and salt that much in the same time so for me it is a time/reward thing to not go this far."

In the picture below from white, he took his tan mescaline and re-crystallized it using the method above with 80%MEK/20%ISO/ water to taste. Absolutely amazing, a milestone actually. Never before have I seen crystal clear mescaline hcl like this. I'll give it a shot one day soon when I'm not so busy. So there you have it, the latest & last word on re-crystallization. I've described several different ways of re-crystallization of mescaline hcl for the purist.

As White mentions at the beginning of this post, all you really need to do is the boiling ETOH (everclear) wash to get some nice product--the boiling ETOH drives off any solvent fumes and leaves you with nice clean product. Re-crystallization takes practice and time.

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#46 tregar

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Posted 08 November 2007 - 04:17 PM

Gringo Biloba said:

Also, a couple of hot acetone washes to the final salt should clean it up quite a bit as well.


Yes, hot acetone works well for cleaning sanchez!

PB:

I use boiling acetone to clean sanchez, it doesn't seem to dissolve (or very little of it anyway).

I was under the assumption that mesc salts were pretty much insoluble in acetone and that the water in non-anhydrous acetone was mostly responsible for mesc solubility.

I usually use about 100ml of acetone to clean 5g of sanchez, and boil it on a lab hotplate. I do let it cool before drawing off the acetone, but there is no visible difference in the level of sanchez when its boiling, or ice cold.


As a matter of fact, I'm getting ready to clean mine with hot acetone, using the funnel/cotton ball technique I posted above, with a hot water rinse in the end of the dried cotton ball into the drying pyrex dish under a fan.

While I'm compiling re-crystallization methods in this thread, here's one from Caljet666 from an earlier post here at mycotopia:

Caljet666 listed this method:

This method cleans most phenethylamines extremely well. You will lose a little product doing this but SWIM reckons purity is the most important aspect of his drugs.

Methyl ethyl keytone is NP but it forms an azetrope with water meaning it will hold a little water. When MEK is bought over the counter as plumb weld primer it has water in it. Acetone does as well and is the reason people lose product when rinsing with it. The water in the MEK is going to be usefull to clean up Mescaline.

Place your Mescaline HCl in a beaker. Add just enough MEK to dissolve it. Put the beaker on a hotplate and bring to a vigorous boil. Use the minimum heat it takes to achieve vigorous boiling.

SAFETY NOTE: Always be careful when boiling flammable liquids. Only use laboratory hotplates or you can modify one from you local dollar store. The thermostats in them work by expanding and contracting metal which can cause a spark when it turns on and off. Solder it closed and put light dimmer switch in the power line. Probably be good to get a professional to put it in. Do it yourself at your own risk.

Boil the MEK until you start to see signs of saturation. You will know its saturated when little crystal start forming on the side of the beaker. Remove it from the heat and put it in the freezer until it is ice cold. Overnight is overkill but SWIM loves overkill in this situation.

When you remove it from the freezer the MEK will be yellow or brown and there will be crystals in the solution. Filter these out. SWIM always uses vacuum filter.

Rinse the crystals with ice cold anhydrous acetone. To make the acetone anhydrous (remove the water) bake some epsom salts in the oven at high temp for a couple hours. They will turn white. When it cools down crush it up a little. Throw a few hand fulls in your tin of acetone. Leave it for an hour or two and shake it every few minutes. Filter the acetone a few times before you use any.

After the crystals are rinsed dissolve them in minimal boiling hot dH2O and evap. SWIM always does this after acetone rinses to remove any remaining acetone so as to not endanger anyone whos predeliction is towards IV.

Comparison of mescaline salts:

Hydrochloric acid is a gas, so excess acid evaporates off, but sulphuric acid is a liquid so, you have to precipitate the alkaloids out of the solution rather then evaporate and scrape.

If you want to use sulphuric acid, then you need to do a titration with an accurate pH meter and dilute sulphuric acid solution. The advantage is you get needle point crystals of a very high purity. These are large crystals and easy to filter out. Mescaline sulphate is not very soluble in cold water solutions so if the solution is pretty cold and spiked with acetone to stop the water freezing, then this is an efficient and easy way of getting the crystals out. The main disadvantages are, you need to dose slightly higher, and if you boil down solutions mescaline and sulphuric acid too far, then the concentrated sulphuric acid will damage the mescaline.

Using hydrochloric acid to salt the mescaline has 3 main advantages over sulphuric acid saltings. 1.) The excess gas evaporates off along with the last of the water, so accurate pH control is not necessary and you can do this without needing a pH meter. 2.) You can gas the non-polar solvent with dry HCl gas, and cause direct precipitation of the mescaline hydrochloride salt. 3.) If you purify the mescaline.hcl enough, then it can be smoked. The main disadvantages of mescaline.hcl are the crystals are tiny and filtration of the HCl gassed non-polar solvent might not catch all of them. This can be helped by spiking the non-polar solvent with acetone before the gassing. But generally using HCl involves the step of evaporating off the water and scraping up the mescaline.hcl.

Refer to Chapter 13 "Recrystallization" pages 119 to 133 for an excellent description of how to re-crystallize with pictures from the book The Organic Chem Lab Survival Manual by James W. Zubrick. You will need a lab hot plate or similar, your solvent and product, and an Erlenmeyer flask, not a beaker. "If you recrystallize compounds in beakers, you may find the solid climbing the walls of the beaker to get at you as a reminder. A 125ml Erlenmeyer usually works."

#47 mate0x

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Posted 09 November 2007 - 01:36 AM

Kick ass thread.... I am ready to try this this weekend. My only question is... I am searching on the HD website and cannot seem to find the watts a-300a barb. Is it something they will definitely have? or I am gonna make a stop at ace as well.... they should carry it? Don't to be wandering around as I'm sure most of the employees will have no idea what I'm talking about if asked at HD.

Very excited to try the gassing technique...I made it through orgo II in college, and I love kitchen chemistry :-) This is by far the most interesting way to do a mesc extraction I have seen.

#48 tregar

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Posted 09 November 2007 - 06:06 AM

Thanks.

There's a lot of stuff that won't show up on their website, just walk around, you'll find it easily in house.

#49 mate0x

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Posted 09 November 2007 - 10:56 AM

Roger that :-)

Going to break it down too, so I can do 4 xylene pulls simultaneously (smaller amounts in 4 different containers....twice each) Should work rather well?

Maybe combine after the 8 small pulls are done... and try a 9th after a few days? Possibly not worth it....

#50 Myco-Iggy

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Posted 09 November 2007 - 06:40 PM

Yea, so despite a few complications...
I think I might have done good :eusa_eh:

The HCl salts were formed by gas,
Caught with water but once seperate, lots of color :mistrust:

I evaped at 200*F and scraped to get a cruddy green Xstal.

Warm acetone seems to have helped alot.
Should find out just how well it was cleaned.

I like the new method, but Ill probably do a titration since I got the equipment still from last try with my next kilo.
After collecting the Xstals in water from the solvent, titrate, then a slow simmer down + filter then carbon/boil and filter
did an amazing hands off job of cleaning.

I want to try the IPA/dH2O ReXstal to see how well the cream colored stuff can still be cleaned.

1.3 from half of a 500g extraction, will finish the other half and try cleaning the cream.

Thanks for all the help!!! Ive learned alot on cleaning.
:bow:

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#51 tregar

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Posted 09 November 2007 - 07:36 PM

Welcome MateOx...good to see you. This is good chemistry practice in lab techniques, learning about re-crystallization process, drying solvents, vacuum filtering, etc.

It is roughly 98% mescaline HCl. Even if green and ugly. when you filter the stuff, the green stained toluene sticks to the powder and stains it. Its unavoidable unless you have a centrifuge.

I used xylene, so mine turned a bright yellow color. Which did you use xylene or toluene?

**That's really strange that when you collected with water, that the water turned green! I've never had that happen, usually the water stays "crystal clear" or takes on a tiny tint of yellow--but only on the 4rth pull. But I did use a sep funnel: I added my gased xylene to the sep funnel, then poured in some hot water, let it sit for 15 seconds, then drained off the bottom water layer which was always clear. Did you use a sep funnel? If you pour your gassed xylene into a sep funnel, then add 1/2 cup of boiling hot water, the water stays crystal clear as it pulls only the mescaline from the solution in the sep funnel, it will be your bottom layer and should be clear, not green or yellow water. It might have a very slight tinge of yellow, but not much at all.

Everytime I've gassed my non-polar (dried xylene) it turned a bright yellow color and not green.

Anyhow, it looks like your acetone wash worked just fine...what I would do now is experiment with re-crystallization techniques to get beautiful pure white or crystal clear mescaline hcl, just like you said you would work on. It looks like you were able to remove the stained nonpolar color from the mescaline hcl.

If this method doesn't work for you, then yes, there's always titration you can do next time.

Anyhow, Let's concentrate on the re-crystallization: I have some good stuff to post on this in the next post. There's where the real magic is at: whether you gas or titrate or do the standard extraction posted by ekstaza/waylitjim, if you re-crystallize your product, it can come out pure white or see thru clear. Gassing your product just gets you a little closer to a cleaner product, so only a 1st pass re-crystallization should yield beautiful perfect product...it will take usually 1 to 2 re-crystallization passes on product from the standard titration or other salting to get to perfect product.

I'm going to be re-crystallizing my product to get it crystal clear using white's method (it does work) of 80% mek, 20% iso, water to taste...

or I will follow the simple mek-recrystallization on post #47 . It should work as there is some water in the mek. I'm pull out my lab hot plate in a couple weeks.

Both methods are "dual-solvent" recrystallizations.

Good job. I'll be posting some new badass re-crystallization stuff in a little bit.

Thanks so much for the pics too. The only reason I can think that your stuff turned green after you gassed it was because either:

1) you used toluene instead of xylene, doesn't matter which you use.

2) "over-gassing" might be the cause of green stained product, but it is easily washed away.

3) the non-polar was not dried with dried epsom salts for about 1/2 hour or more.

4) You gassed your xylene solution, but then did not bubble air thru it with an aquarium pump for 5 to 30 minutes to "bleed" off any excess hcl gas in the non-polar.

How did the gassing go? Did you find it easy? How many times did you submerge the wand in the non-polar and gass it? About 5 to 10 times?

Also, you may find that you get a much cleaner product by using a sep funnel...pour your gassed xylene into the sep funnel, and allow the mescaline to fall to the bottom over a period of 30 minutes...it will all collect at the bottom, from this point on you have 2 options:

1) Option #1 is to collect with boiling hot water....pour your boiling hot water into the sep funnel, then it will collect on the bottom and pull your mescaline out...drain it all out within 30 seconds or so, then put it into a pyrex brownie dish, evaporate off the water overnight, then scrape it up and clean it with an acetone wash.
-------------------------------------------------------------------------------------------
2) Option #2 will give you very clean product....pour your gassed xylene solution into the sep funnel, and wait 30 minutes for all the mescaline to fall and collect at the bottom of the sep funnel.

Then just drain out the bottom mescaline layer: it will be a bright yellow color if you did everything correctly. It might be green like you got. It will be a brown puddle if you did not correctly dry your nonpolar. It's all good.

Then just follow these instructions to get beautiful white product (I have done it this way, and it does work):

See post gass cleanup instructions and acetone/water re-crystallization on post #45.
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Anyhow, in a few hours I'll be posting all of the known re-crystallization techniques that have been used sucessfully with mescaline hcl to get beautiful pure white to crystal clear (see-thru) product with no impurities. Re-crystallization is more an artform than a science, but it gives you potent clean product with virtually no body-load. Whether you salt your mescaline freebase by gassing, titration, or other methods to arrive at your mescaline hcl, it can be cleaned further to yield beautiful product by the magic of dual solvent re-crystallization--it removes the impurities from the crystals yielding a beautiful pure crystalline matrix that grows over a 24 hour period from tiny crystals to large clean crystal matrix, leaving the colored impurities behind in the solvent which you just pour off or filter the whole solution thru a buchner funnel, it will leave your pure crystals on the top of the filter, then just rinse your crystals with some cold acetone. You let your re-crystallization solution cool from boiling down to room temperature, then you put it in the fridge, then you put it in the freezer...a day later you have clean crystals with no impurities.

#52 tregar

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Posted 09 November 2007 - 08:33 PM

This is the alternate way of collecting your product from your sep funnel if you don't want to collect with water. I did it this alternate way to show you how nice it comes out...

1.) On the left is a picture of my dry xylene containing mescaline freebase after it was gassed. Note the bright yellow color of the mescaline and xylene stained yellow at the bottom that collects around the crystals. This is normal.
2.) Pour the jar into a sep funnel.
3.) Wait 30 minutes, and all of the yellow stained mescaline hcl will collect at the bottom of the sep.
4.) Drain out the yellow stained mescaline into a buchner cup with a filter disc and put it on a buchner funnel vacuum setup.
5.) Clean it with acetone and rinse with more acetone (at least 3 times) following avalo's post gass cleanup on post #45, I've also re-posted it below.
6.) This is a pic of the yellow goo ball that drops out of the lower part of the sep funnel...after a while the xylene evaporates off the product, but as it's evaporating you can see white mescaline oozing out of it and collecting on the dish.
7.) The yellow goo ball must be cleaned and rinsed with acetone on a buchner cup following avalo's procedure here: Then you must use boiling hot water/acetone re-crystallization to drive off the solvent fumes from the white mescaline...this also gets it crystalline pure. Here's the procedure you follow:

Part I, Post Gassing Clean-up

Filter the mescaline.hcl from the gassed xylene with a buchner funnel & vacuum. (or if you put it into a sep funnel, it will be the lower bright yellow layer, just drain it out into a small puddle). Wait a little white for the xylene to evaporate off the powder.

Then wash the powder with clean xylene. This flushes through any brown cactus crap that was also in the xylene.

Now disconnect the vacuum hose to break the vacuum. Then reattach it, but leave the vacuum turned off. This creates a sealed volume of air, so when you pour liquid on top of the filter paper, the trapped air will tend to keep it there instead of allowing it to drain through.

Now using a wash bottle, wash the powder with acetone until it's completely covered, and let it sit for a couple of minutes. Then turn the vacuum on, and filter through the acetone. Now rinse the powder with more acetone as it's being sucked through. This soaking and washing will remove the vast majority of the xylene.

Cover the filter funnel with a large oversized piece of filter paper, and suck air through the funnel for a couple of minutes, this will help dry the powder and protect it from dust.

Now remove the filter funnel and allow the white powder to completely dry.

Once dry, the power will flake off the filter paper, so you won't get mushy paper fibres in with your product. (tregar: see post #54, that's a picture of the whiteness the gassed product will be after doing this simple fast acetone cleaning): but it's still not done yet--it has solvent fumes/residue that must be "driven" off by adding it to boiling hot water, the next step.


Part II, Acetone/Water Recrystallisation

Place the mescaline.hcl powder in small 50 mL Erlenmeyer flask.

Use hot distilled water to soak the filter paper, and wash the filter funnel.
Add this to the flask, and then add a small boiling chip.

Using a lab hot plate or oil bath, boil the water down until it starts to get a sheen on the surface.
The boiling water will drive off any residual solvent vapours, and you boil it until the mescaline gets concentrated.

Then remove it from the heat, and let it cool down a bit. If crystals start forming immediately, then you've boiled off too much water. So add a bit more water then re-heat it and boil it down again.

Once the solution is concentrated and warm but not hot, then add an equal volume of acetone. Crystals should start forming immediately.

If the crystals don't form when you add the acetone, then there was too much water in there, so boil it down again. The acetone will all boil off first, then boil off a bit more water before letting it cool and re-adding some more acetone.

Once you add the acetone and the crystals start forming, then reheat it, and drip in a single drop of water at a time, until all the crystals dissolve in the hot acetone/water solution.

Then remove the boiling chip and let the solution slowly cool down to room temperature, then place it in the fridge.

Filter the pure crystals out.

You can also recover the mescaline traces and impurities by evaporating off the waste liquid on a Pyrex dish.

The recrystallisation is a bit of mucking about, and I hear it takes practice to master, I've only read about this at the moment. But the trick is to get the crystals to grow out of the solution as it cools. If you crash the crystals out too soon, then they form small crystals that grow very fast and trap impurities inside the crystal matrix.

The other thing you can do to remove solvent residue is put your powder or crystals in a short test tube and place them inside a filter flask. Put a solid bung in the top and then turn the vacuum on. The reduced pressure makes the solvents evaporate off much more quickly.

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#53 tregar

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Posted 09 November 2007 - 08:50 PM

See the yellow goo ball on the top post? Well, after you wash it with acetone and rinse it with acetone, it looks like this--very white--the picture you see below is when I took the white wet filter disc from the buchner after the washing and rinsing with acetone (took 5 minutes or so) and plopped it into a vacant dish...as the last of the acetone evaporated from the mescaline, it coated the entire dish, so I scraped it up to get it ready for the next step...now you just follow the water/acetone re-crystallization steps above (part II) to drive off solvent fumes and get it pure as can be.

The bright yellow color washes away from the gassed product VERY EASILY and QUICKLY with acetone as you can tell. The product is indeed white, but it is not done yet! It needs to be added to boiling hot water to drive off any solvent fumes--this will eliminate all chemical residue, taste and smell from the product. Just follow avalo's boiling hot water/acetone re-crystallization above (part II) or another method of re-crystallization of your choosing.

Myco-Iggy is dreaming about doing the IPA/water re-crystallization process, that's another great method you can substitute in place of part II above...there are many different re-crystallization methods you can use.

I'll post some more good re-crystallization methods later that may be easier. Even if you used a different method of salting out your mescaline, such as waylitjim's method or a different method and ended up with very brown, brown, or tan product, you can do a re-crystallization on it to get some pure looking stuff...re-crystallization will remove the impurities from very brown, brown, tan, off-white or white mescaline.

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#54 tregar

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Posted 09 November 2007 - 11:36 PM

Ok, here it is, what I've promised...

THE ULTIMATE COMPILATION OF DUAL and TRIPLE SOLVENT RE-CRYSTALLIZATION METHODS for mescaline hcl:

I'm going to list and describe all the details of 4 popular methods below...also don't forget the 5th method above by avalo (part II) on post #53. Study and pick the re-crystallization method you like the most....experiment till you find the one you like the best. Once you read all the methods in this post, you will see how similar they are and have a better overall understanding of re-crystallization.

Refer to Chapter 13 "Recrystallization" pages 119 to 133 for an excellent description of how to re-crystallize with pictures from the book The Organic Chem Lab Survival Manual by James W. Zubrick. You will need a lab hot plate or similar (no flames), your solvent and product, and an Erlenmeyer flask, not a beaker. "If you recrystallize compounds in beakers, you may find the solid climbing the walls of the beaker to get at you as a reminder. A 125ml Erlenmeyer usually works."

I'm very interested in re-crystallizing my small amount of powder. I just so happen to be very sensitive to impurities, and just plain like re-crystallizing stuff now that I've read so much on it...I'll post pics in a few weeks of the results before and after. I don't care if it takes 1/2 a day to do or more...1 pass should do it with the gassed product I believe. I was very impressed with white's photos of the before and after: before: 1500mg opal tan, after 1234mg crystalling translucent mescaline hcl. me!'s hcl crystals are just as mind-blowing. Like me! saids, the re-crystallized product has no perceptable body load, very clear.

These are some questions I asked white:

What were the approximate amounts of 80% MEK and 20% of the 99% ISO that you used for the 1500 opal tan? I'm going to try this in a couple weeks, just waiting on a real lab hotplate I've decide to go with.

Question 1) You used 10x the volume solvent to product as fine powder. So if you have 1500mg powder, how much MEK would that be? How much ISO would that be? I'm not good at this kind of conversion.

Question 2) Do you think there is a bigger advantage to using MEK with ISO together as opposed to MEK by itself?

Question 3) You used non-dried MEK right out of the can right? Just checking to make sure.

Question 4) What do you think of method 2 below by Unknown? It works because MEK has some water in it, so it's a dual solvent re-crystallization. Do you think it will work as posted? It looks like a nice method for a beginner.

Question 5) What do you think of method 3 by me! ??

Because, in me!'s method he used 150ml of boiling hot MEK to 3 grams of mescaline hcl.

However, avalo saids to use 100mL of boiling hot DRY MEK per 1 gram mescaline powder.

Who's right? I'm just a little confused...

me! saids:

The solubility of the HCl salt in water is right around 700 mg/cc in warm (but not boiling) water. give or take as much as 50 mg... the actual solubility is slightly higher than this, but 700 is approaching saturation...

solubility in boiling mek is more like 1000 mg to 150 cc or 6.7 mg/cc...

solubility in boiling IPA is in between but much, much closer to water... like 500 mg/cc or thereabouts.

solubility in methanol is closest to water, followed by ethanol then IPA... (makes sense... order of polarity...)

the figures for water are pretty good. the ones for mek and IPA are ballpark figures, but pretty close to accurate..

1) White's excellent method (see pic of his translucent mescaline hcl earlier in this thread):

I gave this a go using 99% iso.First attempt used too little solvent and ended up with a chunk in the freezer so redid it with 5x by volume iso and brought to heat this nearly disolved it completely. I added only one drop of water and it cleared I reduced it until it "shimmered" and cooled slowly to recover a thick layer of clear-tan xtalsfrom the alcohol these were xylene washed to remove even more "color" then boiled in etOH to clear all solvents and dried to the same color as tregars gassed product ( pics when camera gets some batteries).

Results; MEK/Iso/H2O is much more efficient at collecting impurities and trapping them while releasing the alkaloid in a more pure state .Iso/water returned only 74% of the product as crystaline and held over 25% in solution after freeze precipitation it also left more color than the MEK/Iso/H2O method which generaly returns high 80 to mid ninty percent of my "crude" as off white Xtals.

80%MEK/20%ISO/ water to taste.Dropwise until it reaches shimmerosity then one or two past till just barely clear, boil until just shimmering again and slow cool.
I use 10x by volume solvent to product as fine powder.
for very clean linen white product repeat process then slow crystalize from etOH for clear needles. Pics below.

That was just for show. It can be done to perfection. For me however this is wasteful of my time and effort as the opal tan from a 'tone wash and etOH boil is as good as I need. Just wanted to show what CAN be done with practice and if it is that important to you. 'Tone ,MEK and MIBK will all work as will etOH in place of ISO but the 95% etOH I get you dropper in after10% due to the 5% H2O.
1500mg opal tan yielded 1234mg of the clear crystals pictured after two passes and an etOH boil

2) Method "2" by Unknown:

This method cleans most phenethylamines extremely well. You will lose a little product doing this but SWIM reckons purity is the most important aspect of his drugs.

Methyl ethyl keytone is NP but it forms an azetrope with water meaning it will hold a little water. When MEK is bought over the counter as plumb weld primer it has water in it. Acetone does as well and is the reason people lose product when rinsing with it. The water in the MEK is going to be usefull to clean up Mescaline.

Place your Mescaline HCl in a beaker. Add just enough MEK to dissolve it. Put the beaker on a hotplate and bring to a vigorous boil. Use the minimum heat it takes to achieve vigorous boiling.

SAFETY NOTE: Always be careful when boiling flammable liquids. Only use laboratory hotplates or you can modify one from you local dollar store. The thermostats in them work by expanding and contracting metal which can cause a spark when it turns on and off. Solder it closed and put light dimmer switch in the power line. Probably be good to get a professional to put it in. Do it yourself at your own risk.

Boil the MEK until you start to see signs of saturation. You will know its saturated when little crystal start forming on the side of the beaker. Remove it from the heat and put it in the freezer until it is ice cold. Overnight is overkill but SWIM loves overkill in this situation.

When you remove it from the freezer the MEK will be yellow or brown and there will be crystals in the solution. Filter these out. SWIM always uses vacuum filter.

Rinse the crystals with ice cold anhydrous acetone. To make the acetone anhydrous (remove the water) bake some epsom salts in the oven at high temp for a couple hours. They will turn white. When it cools down crush it up a little. Throw a few hand fulls in your tin of acetone. Leave it for an hour or two and shake it every few minutes. Filter the acetone a few times before you use any.

After the crystals are rinsed dissolve them in minimal boiling hot dH2O and evap. SWIM always does this after acetone rinses to remove any remaining acetone so as to not endanger anyone whos predeliction is towards IV.

3) Method 3 by me! (excellent white to translucent product):

Approximately 3 grams of naturally occurring white mescaline HCl that had been previously produced by gassing was added to 150 ml of boiling methyl ethyl ketone. The ketone was allowed to boil vigorously but was observed to be clouded by undissolved material. Distilled water was added by dropwise addition until the clouding cleared. The material was boiled down until the solvent just began to display signs of saturation, at which time, it was removed from the heat, covered and transferred to a freezer. At the conclusion of two hours time, the beaker was removed from the freezer and observed to be filled with a golden colored liquid saturated by a massive conglomeration of a material that bore uncanny resemblance to sparkling clean crushed ice. The contents of the beaker were fast filtered through a vacuum funnel and rinsed with very anhydrous ice cold mek followed ice cold anhydrous acetone. After subsequently stripping any residual solvent under vacuum, the material was observed to display spectacular clear needle formations, each roughly .10 mm in length.

The bulk of this material was subsequently dissolved in a minimum of boiling distilled water and the volume of the solution reduced to just above saturation. At this time, the beaker was removed from the heat and placed on the lab bench for observation. It was immediately noticed that a thin skin of crystals had appeared around the upper interface between the walls of the beaker and the mescaline liquor. Within seconds, the skin began to expand radially inward at a rate of very roughly .2 mm/sec. Simultaneous to the skin moving across the surface of the liquid, an amazing array of fractal patterns appeared in its wake, frozen in the crystal. After an hour, the beaker was observed to be filled with long dagger shaped crystals that lay parallel to the base of the vessel. It was then flooded with anhydrous acetone and the crystals broken free into a suitable vacuum funnel. Upon drying under vacuum, the material assumed the appearance of very large white/clear shards of mescaline hydrochloride.

me! in depth on the above process:

Of course one can do the boil outside and then bring it inside to put it in the freezer... this isnt such a bad idea as boiling mek reeks pretty badly... swim happens to rather like the smell of mek, but nobody he's ever lived with shares in his strange love for the smell of boiling ketones and these kinds of experiments have caused more than one domestic dispute in swim's house... also, ketone solvents such as mek and acetone are quite flammable, so doing this outdoors adds a measure of safety in that the vapors wont concentrate in a small space... one needs copious ventilation when doing this indoors to avoid risk of fire or being overcome by the vapors... this isn't really that big of a deal when working with small samples but the smell is very extremely disagreeable to many, if not most people... doing this outdoors really is a good idea providing one can do so without some busybody snooping on his activities and calling the cops...

what happens with this is that mescaline HCl is not terribly soluble in mek, boiling or not... the "cloudiness" that swim mentions is caused by the undissolved mescaline clouding the solution... one simply adds water in very, very small increments until the solution ceases to be clouded by any undissolved mescaline... just a few drops at a time, little by little until the liquid turns clear... the water simply causes all of the mescaline to go ahead and dissolve... then one just boils it down until he notices it taking on a "shiny" appearance... think of something like silver or gold paint that has been sitting for a very long time --- this kind of paint will often seperate, with the solid part going to the bottom and the solvent floating to the top... now imagine taking a stick and very gently stirring it so as to bring some of the solids up into the solvent layer... you will see a metallic shimmering "swirl" in the wake of the stick you are stirring it with --- this is exactly the sort of "shimmer" swim is refering to with the mescaline... its not as bright, of course, as the aluminum powder that makes the metallic paint shimmer and sparkle but it looks very, very similar... this is what you are looking for... when you see it begin to appear this way that is when to put it in the freezer... give it about an hour or two in the freezer --- if nothing happens (i mean if no crystallization occurs) in 2 hours time, it only means you did not boil it down far enough... just return it to the heat and boil it down a little further and then put it in the freezer again... you might have to boil it two or three times (especially if you have never done an mek crystallization before) but just keep returning it to the heat and boiling it a little more and then putting it back in the freezer until it crystallizes... once you find the "sweet spot" the first time, it will be exceptionally easy to find it in subsequent experiments... its not in the slightest bit difficult but like I said, if the process is unfamiliar to you it might take a couple of tries to get it boiled down to the right concentration for crystallization to occur... the nice thing about this sort of technique is that it is nearly impossible to damage your product unless you boil it down to tar and let it overheat and burn it...

to further understand the process, swim strongly recommends studying swigeezmiester's recent thread on the technique as applied to pseudoephedrine HCl...

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

do, of course bear in mind that swigeeze is writing about pseudoephedrine HCl and not mescaline HCl so many of the fine details are not going to directly apply, but the underlying mechanisms and techniques are identical --- the exact amounts of solvents and legths of time and such that geez speaks of are not going to be the same at all with mescaline but the theory is identical and his write up is the most comprehensive and complete description of the technique swim has come across so far... it will assist you greatly in understanding what exactly is going on...

swim himself developed the mescaline/mek technique out of repeated experiments with mek crystallizations of pseudoephedrine and *************** and is of the opinion that this sort of crystallization regime will work on any hydrochloride phenethylamine salt although he has not attempted it with any of these compounds except for hydrochloride salts of pseudoephedrine, ***************, ephedrine and mescaline... it works exactly the same with each of these with the differences being only in the relative amounts of polar solvent (water, methanol or other alcohol) that one uses...

also, you will notice that swigeeze employs methanol and references the use of other alcohols in place of water in his write up... swim has not tried any of these with mescaline, but can think of no reason whatsoever that they will not work with this phenethylamine as well... bear in mind, that swigeeze is working with material that has been deliberately adulterated with exceedingly difficult to remove agents added to thwart efforts at purification... while the cactus does contain natural agents that behave in very similar fashion to some of these gaaks, the naturally occuring impurities in the cactus are nowhere near as tenacious as the human engineered ones present in pseudoephedrine pills and do not require anywhere near as much precision to remove...

in particular, swim's mescaline experiments have not required boiling the material down quite as far as what swigeeze mentions with pseudoephedrine although swim can find no reason that boiling it down this far would in any way result in a substandard product... its just not the exact way swim did the experiments...

(bear in mind that mek crystallization of mescaline is pretty much uncharted territory and the final word on the topic is far, far from being written... just play with it and see what swiyou comes up with... you really cant go wrong... even if you find you must abort the experiements for whatever reason, dont worry about losing your product --- simply evaporate the mek off the product and it will return to you exactly as it was before you dumped it into the mek...

(swigeez spared no effort at presenting a highly comprehensive description of what his research has revealed and it could appear overwhelming to one not used to this sort of chemistry (purification of pseudoephedrine from denatured OTC preparations)... but a rigorous study of his write up cannot fail to provide you with a much more comprehensive understanding of the technique and why it works...)

as far as the differences between highly pure crystalline mescaline HCl and crude brown impurity laden mescaline HCl... first and foremost, pay no attention whatsoever to those who claim there is no difference or to those who claim the impure stuff has a better effect...

swim has been arguing with these luddites for a number of years now and knows many of them personally... the honest truth seems to be that the majority of them are offended by a **** cook using techniques perfected and developed in the **** lab on mescaline... there is a certain segment of the clandestine chemistry community (those who like to toss around nonsensical words such as "entheogen" and such...) who believe that **** is evil and that anything we ********* develop is also spiritually on the wrong side of the fence... seems they believe that a product produced in a mason jar with the most egregiously ghetto of possible methods is more "spiritual" than a product produced by more advanced means...

I would counter that the Creator endowed me with my intellect and my ability to utilize and develop tools to better survive in my environment and to refuse to make full use of all that has been made available to me is the grossest of insults to that which Created me! The prehistoric Shaman who first ground up a cactus between two rocks and boiled it in a clay pot with water and lemon juice was utilizing the full scope of the technology available to him at the time... one can best believe that had he had access to such things as mek, he would surely have used it! There is nothing inherantly spiritual about crude prehistoric technology that is not present in modern technology...

the simple fact of the matter is that the more pure a given drug becomes the safer it becomes for the end user (more accurate dosing along with the absence of potentially dangerous and unknown impurities translates into greater safety for those who consume the products) and also the more potent it becomes... many people steadfastly believe that there are additional alkaloids present in trichocerus cacti than mescaline, however, long, long experimentation (several years) has convinced swim otherwise... trichocerus cacti do not share the same alkaloid profile with peyote cacti which are know to legitimate science to contain several additional alkaloids, a number of which are known to be psychoactive in one way or another... every indication seems to point to the trichocerus cacti containing but a single alkaloid, mescaline...

swim has not, however, performed TLC or other such direct investigations of the material to verify this... most of the reason he believes as he does is based on observations of the melting points of very highly purified samples of trichocerus based mescaline... swim has successfully produced samples that routinely and predictably melt within fractions of a degree of published known values for the alkaloid... were additional alkaloids presnt, crystallization alone would not seperate them (chromatography or other such advanced methods would be required) from one another and the resulting products' melting points would be divergant from published values for the pure substance...

just as certain impurities in *************** can radically modify the percieved effects of the drug, so do impurities modify the percieved effects of mescaline...

swim finds that, as purity of the material increases, body load decreases and the effect becomes more cerebral and more "clear"... above all, same as with *************** HCl, the potency of the material seems to increase exponentially as purity increases... it seems the impurities present do much more than merely throw off the dosing... they seem to invariably inhibit the actions of almost all drugs... true, some impurities in **** seem to intensify the rush but this inevitably comes at a cost of a shorter duration at best or obnoxious and/or unhealthy (even dangerous) side effects at worse... mescaline, being a hallucinogen that shares the same phenethylamine core with the true amphetamines is also something of a stimulant and seems to follow the exact same pattern.

in spite of the volumes swim and others write in attempts to explain this technique, it really is an extremely simple and easy proceedure... much, much more foolproof than regular dual solvent crystalization techniques (ie: those that use water and acetone or an alcohol and acetone...)

Tregar (May, 2007):

Can the sanchez just be added to boiling MEK on a hotplate outside, allowed to cool, then put in freezer for a while till xtals formed, then filtered off under vacuum? Or is there more to it than that, what is with the adding of distilled water to get out cloudiness...don't understand any of that.

Avalo (May, 2007): Excellent answer, thanks so much for this Avalo, learned alot. NOW I understand.

No, that wouldn't work because mescaline.hcl is practically insoluble in MEK, but it is soluble in water. The MEK thing is a dual solvent recrystalisation: MEK and water. The impurities are soluble in both water and mescaline, but are slightly more soluble in MEK then the mescaline is. That's why the mescaline will drop out first.

This has to be done quite precisely because if you add too much water, then not all your mescaline will precipitate out. But if you don't add enough water, then the impurities stay stuck to mescaline powder instead of dissolving into the solution. So you have to use well dried MEK, and once it's boiling, you add 1 drop of water at a time, just until all the mescaline powder dissolves. This gets both the impurities and the mescaline dissolved in the MEK/water mix. And then the solution becomes clear instead of shimmery. It would help if you could stir the solution with a glass rod in between water drop additions, as this helps get everything mixed round well, and would help to avoid adding too much water.

After getting the mescaline powder to dissolve, you boiling the solution to drive off the water (along with some of the MEK) until the solution becomes saturated (shimmery again). The loss of some of the water is what makes some of the mescaline precipitates out as tiny seed crystals. When the solution is cooled down, the rest of the mescaline grows on those crystals, forming large ones. The impurities stay in the solution.

4) method "4" by persona:

Personally, I would go with a more defined recrystallization. The easiest thing to do would be to Isolate your crystals as per the method given, and recrystallize from USP grade 91% isopropanol and dH2O. Using these two would ensure purity. Put your crystals in a beaker, heat isopropanol on a water bath till a boil, cover the crystals and slowly start adding hot dH2O until they are dissolved (this whole process is done while the isopropanol/water/Mescaline solution is boiling). Then continue heating and add a few drops of room temperature 91% isopropanol, until you start seeing a very very slight film or precipitation develop. Then remove your water bath from the heat, cover it with a towel (with the beaker still in it), and leave it alone and completely undisturbed, in a fairly dust free enviroment until it reaches room temperature and then some few hours on top of that. Stick the whole thing in the fridge very carefully after that, followed by into the freezer. This entire process, if you are patient and do it properly, should take around 24-36 hours. Some fairly spectacular crystals will develop, which you can then used as seed crystals for subsequent crystallizations, which save you a lot of time and also allow for extremely pure crystal formation.

The nice thing is that once you have one seed crystal, you can cut the time needed for recrystallizations quite a bit, and also can ensure purity and quality with 0 worry. Believe me, it's really worth it to try. Try and recrystallizing 1g, it will be worth it.

As far as ratios go, just figure it out experimentally. Heat your solvent and add it slowly to the crystals until they are at least covered. I would say, 5g of crystals in 25-30ml of isopropyl alcohol is reasonable. Then add water from there. It will take some time to figure out the true ideal ratios, but if you understand the concepts behind crystallization it's a cinch.

I should probably mention these now. You want to create a solution that dissolves the Mescaline at boiling, but is relatively insoluble to Mescaline at freezing. You want the impurities (primarily non-polar substances, or amine salts like Mescaline , present in far smaller amounts) to remain soluble in solution.

If you use too much alcohol in beginning, say 100ml per 1g Mescaline , you will just dissolve your crystals at all temperatures, and will need to boil down your alcohol to attain a more proper mix. So if you add too much alcohol, before adding more water, let the alcohol evaporate and then add water.

If you use too much water, you will need to evaporate the solution down a fair amount and then repeat the procedure from start basically. Avoid doing this, always add extra alcohol, not water.

If you need to adjust crystal solubility remember, adding more water dissolves more crystals, so ultimately adding 3ml of water might dissolve an entire gram... at room temperature! You need to add water slowly. If you added too much water, you would want to evaporate the water for a few minutes, then add more alcohol so that the crystals precipitate slightly upon adding the very last drop.

Once you have your idealized solution, let's say, ~90ml ~60/40 isopropanol/water @ 90C dissolves 10g of Mescaline you find, at precipitates 9g at freezing (this is made up so don't actually use this to start, use the above methods)...

You start with 10g Mescaline . You add 91% boiling IPA to the crystals. The beaker that the crystals are in should now be placed in the water bath, and the solvent continued to be boiled. Only a little bit dissolves. Slowly you add water in premeasured portions, say 1ml per addition, until the Mescaline dissolves. So assuming you started with 60ml of 91% isopropanol, you find that after adding 27ml of dH2O dissolves all the Mescaline at boiling point - specifically, you add the last drop and the last of the crystals go into solution. You heat the mixture to a vigorous boil, add another drop of isopropanol, then carefully cover and allow it to sit. After freezing you collect 9g of crystals. You evaporate your mother liquor until crystals precipitate and repeat the procedure to collect another .9g. Just remember, each subsequent collection past the first is more and more impure - so adjust the rations properly right away.

Once you collected and weighed, you can calculate the actual proportions. (That is, you of course won't know that 60/40 is the ideal mix, only after when you see that you added with much water to your solvent etc...).

Anyway, some fairly involved procedures, but really worth it. Try it on a gram or two, you won't regret it!

Remember, if you screw up, you can just evaporate your solvents and recover your product.


RANDOM RE-CRYSTALLIZATION WISDOM:

me! (November 2006):

I 've been mentioning the use of isopropyl alcohol as a crystalization solvent for how long now? 2 years maybe?

it does work but nowhere near as reliably nor as cleanly as mek.

IPA only works marginally well with nasty sanchez.

mek will turn even greenish black slimy sanchez into clear crystal in an hour's time.

ipa is better suited as a second pass crystalization solvent.

Rhodium:

1) One good way for ensuring that your alcohol cools down nice and slow is to put some water in a pot and heat it to boiling and take it off of the heat. Then put your container with hot alcohol/dissolved crystals in the pot of water being sure not to get any water into the alcohol, cover the container, and let it cool down to room temperature. Then you can put the container with alcohol in the refridgerator to cool more. Then into the freezer to cool more. Then you can filter your pretty crystals out. Now there is usually still a little bit of product left in the alcohol, so if you boil off say 75% of the alcohol and repeat the cooling process you can get some more crystals. The slower the rate of cooling, the bigger the crystals formed.

2) The most common method of purifying solid organic compounds is by recrystallization. In this technique, an impure solid compound is dissolved in a solvent and then allowed to slowly crystallize out as the solution cools. As the compound crystallizes from the solution, the molecules of the other compounds dissolved in solution are excluded from the growing crystal lattice, giving a pure solid.

3) Crystallization of a solid is not the same as precipitation of a solid. In crystallization, there is a slow, selective formation of the crystal framework resulting in a pure compound. In precipitation, there is a rapid formation of a solid from a solution that usually produces an amorphous solid containing many trapped impurities within the solid's crystal framework. For this reason, experimental procedures that produce a solid product by precipitation always include a final recrystallization step to give the pure compound.

4) Once a suitable solvent is selected, place the impure solid in an Erlenmeyer flask and add a small volume of hot solvent to the flask. Erlenmeyer flasks are preferred over beakers for recrystallization because the conical shape of an Erlenmeyer flask decreases the amount of solvent lost to evaporation during heating, prevents the formation of a crust around the sides of the glass, and makes it easier to swirl the hot solution while dissolving the solid without splashing it out of the flask.

Keep the solution in the Erlenmeyer flask warm on a hot plate or in a water bath, and add small volumes of hot solvent to the flask until all of the solid just dissolves.

5) Sometimes the dissolved compound fails to crystallize from the solution on cooling. If this happens, crystallization can be induced by various methods. One way to induce crystallization is by scratching the inner wall of the Erlenmeyer flask with a glass stirring rod. This is believed to release very small particles of glass which act as nuclei for crystal growth. Another method of inducing crystallization is to add a small crystal of the desired compound, called a seed crystal, to the solution. Again, this seed crystal acts as a template on which the dissolved solid will begin crystallizing. If neither of these two techniques results in crystallization, the compound was probably dissolved in too much hot solvent. If you believe that you may have too much solvent for the amount of dissolved compound, reheat the solution to boiling, boil off or distill some of the solvent, and then allow the solution to cool to room temperature again to effect crystallization.



#55 tregar

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Posted 10 November 2007 - 07:25 AM

By the way, in answer to question #5 above:

avalo said:

Me!'s right, I was recalling his experiments and I didn't remember correctly. I'd go with Me!'s suggestion of 50 mL MEK per gram of Mescaline. I do remember reading about someone's attempt to do the MEK recrystallisation, and they just got a black solvent and water layer with no crystallisation. The problem was they didn't use enough MEK to hold all the water and impurities, so everything crashed out all together.

But iirc the MEK has to be dried before you use it. This way when you drip in the water, the MEK will be able to hold onto it. MEK is wet straight out of the can, so if you try to drip water into this, then MEK might already be saturated, so the water will just pool on the bottom.

Just a reminder, keep these safety notes in mind from Caljet666 here at mycotopia:

Caution boiling mek is definately a must. I have said this before but it can't be said enough IMO. The thermostat in most electric hotplates can cause a spark when it is turning on or off. Solder it shut and put a light dimmer switch in the power cord.

80 deg C is its boiling point, so that is how hot you want it. Use enough mek that the water in it only just dissolves the mesc while it is boiling, or you could use a little less and add dH2O dropwise until the rest dissolves, again while boiling.

The hot water will dissolve a fair bit of mesc. When you put it in the freezer it won't be able to hold near as much mesc and it will crash out, leaving a most of the crap behind.

Buchner funnels are worth there weight in gold in conjuction with vacuum. If you dont have them, at least filter in the freezer while the solution is still cold.

You could also, if you want, put the mesc in boiling anhydrous mek and add ethanol, iso or some other polar solvent dropwise until it all dissolves.

Different combinations will work against different impurities, however swim finds mek to be the best if you are going to use only 1.

Stay Safe
Peace
Caljet


*Some tips:

*An actual sparkless lab hotplate is the way to go with re-crystallizations.

*You should use a mineral oil bath or skillet/cake plate full of sand or pea gravel with or without some mineral oil mixed into it to sit on top of your lab hotplate, then position your erlenmeyer flask inside the sand or bath for even heating when heating your solvent(s) for the re-crystallization.

*Don't forget that when you boil alcohol in a flask, it needs a boiling stone or a chipped piece of porcelain in there, or as a substitue for that, you can keep your solution spinning the whole time, but remember, as soon as you stop spinning, the alcohol could "shoot out" due to there not being a boiling stone in there, this is necessary when boiling an alcohol.

*A fire extinguisher and a box of baking soda are good to have around, as well as a decent home made fume hood to use with your lab hotplate inside of it. Full set of goggles that go around your eyes, heat & chemical resistant gloves, long sleeve shirt, gas mask when gassing, etc.

*A 1000 mL sep glass sep funnel (about $60 or so) is really needed to do this process, it allows your gassed mescaline to fall and collect at the bottom, so you can drain it out in a puddle easily after 1/2 hour or so...

*It also is needed if you plan to collect with water as an alternate collection method, by adding 1/2 cup boiling hot water to the sep, then wait 15 to 30 seconds, and drain off the lower crystal clear water layer which will pick up the mescaline hcl....evaporate it off under a fan overnight, then scrape it up and clean it with acetone and a hot boiling water rinse through the cotton...then put hot water in a dish, evaporate it off, and scrape it up again.

*Lye (sodium hydroxide) needs to be pure, I wouldn't use drain openers these days, they contain additives, there may be one brand out there that works, but it sure ain't zep 10, it has aluminum. I got my lye from a soap making place a long time ago. There may be one brand out there that's ok to use though.

*muriatic hcl acid comes in jugs at around 31.45% at hardware stores and such for cleaning pools, driveways, etc.

*A 3 gallon glass carboy and stopper can be found at beer making supply houses on-line.

*A buchner funnel and vacuum aspirator for a faucet for generating a vacuum comes in handy too, worth it's weight in gold like Caljet666 saids.

I should have renamed this thread--Crystal Clear Mesc hcl--for the chemist or advanced hobbyist, not "so easy" after all.

If you want an easy tek to follow, follow the one by waylitjim or smacked12 here at the forum, or you could do a titration if you have a good ph meter. By then following one of the re-crystallization procedures in the post above (1 of 5 popular methods), you will then be able to clean up the product (should you wish) from waylitjim's or smacked12's tek: http://mycotopia.net...cl-extract.html

You should be able to do one of their tek's first (and be proficient at the salting steps and subsequent acetone cleaning using a funnel and cotton ball and hot water rinse of the dried cotton) before moving on to this tek.

Pleasant dreams.

#56 tregar

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Posted 11 November 2007 - 07:22 PM

All you really need to know for a kick ass re-crystallization to turn your yellow, tan to off-white looking sanchez into pure white to translucent mescaline:

2 passes may be needed to turn dark brown sanchez into pure translucent product, judging from White's latest experiment. He used 80% MEK, 20% ISO, water to taste. He added 10x the amount of product as solvent. 1 pass will be all that's needed to turn gassed product (as collected above in post #53 & #54) to pure white to translucent product. Even if you collect your gassed mescaline hcl with a sep funnel and hot boiling water (drain water off within 15 seconds or less), you should be able to get pure white to translucent product with 1 pass.

I dont know how to simplify it any more than this. Its easy. Put 3 grams sanchez in erlenmeyer flask with 150 mL boiling mek (a large excess of mek.) Use around 50 mL per 1 gram of sanchez. Put a boiling stone or chipped piece of porcelain in your flask too. Add water drop by drop until all the mescaline dissolves, it will go from a "cloudy" appearance to a "clear" appearance when you have added enough drops of water, this means the last of the mescaline has dissolved. You can stir it a little with a glass rod after each water drop addition to make sure it mixes in well. If your lab hotplate has a built in stirrer, then you can turn on the stirrer for a while after each addition. Then just boil down until the liquid begins to "shimmer" --- it will take on a shiny shimmering appearance. Stick it in the freezer for a couple of hours. If no crystals appear, simply boil it some more and shove it back in the freezer. Once you have crystals, simply filter them off and rinse with cold very anhydrous acetone. Let dry. Add crystals to a minimal amount of boiling hot water in a pyrex brownie dish sitting under a fan to drive off any acetone fumes...When water has evaporated, scrape up the crystals. Eat crystals. Trip balls.

Make sure you use a laboratory style hot plate with a thin skillet or cake plate of sand with or without added mineral oil added to the sand, or an aluminum cup with mineral oil bath to hold your flask...and a fume hood is a must if this is being done inside. See the pictures at the beginning of this post to see how to build an easy fumehood in under 2 hours. You can do this while you watch TV. It mounts up to an open back window. Keep a fire extinguisher on hand, baking soda, a bucket of sand, wet towel, etc. for safety reasons. Don't have any open flames anywhere, not even a pilot light, and don't smoke. Wear full protective goggles, heat resistant chemical gloves, long sleeve shirt. The powerful fans are of the brushless computer PC type, they are non-spark.

#57 tregar

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Posted 11 November 2007 - 07:34 PM

For really big crystals, put the flask in a pot of boiling water that has been taken off the stove and put on a mitten on a table, cover the top of the flask...the pot will take ages to cool down...this will help develop awesome crystals, then when the pot reaches room temp, put your flask in the refridgerator, then move it to the freezer overnight. In the morning you will have tons of beautiful pure white to see-thru transparent crystals depending on how clean your stuff was to start with. The gassing gives you pretty clean stuff anyways, see post #54 for typical color of post gassed product. Your MEK will be brown to gold colored...just filter off your crystals over a #101 to #103 round disc filter sitting in the buchner cup of your vacuum filter flask and rinse them with ice cold anahydrous (dried) acetone.

To make the acetone anahydrous (remove the water) bake a thin layer of epsom salts in the oven at high temp 400 degrees F. for a couple hours. They will turn white. When it cools down crush it up a little, use a spatula to scrape it up. Throw a few hand fulls in your tin of acetone. Leave it for an hour or two and shake it every few minutes. Decant off the top layer of acetone above the rocks and filter it a few times thru a #103 filter disc on a vacuum flask before you use any. If your acetone is anahydrous you won't loose any product when you rinse the crystals.

After the crystals are rinsed dissolve them in minimal boiling hot dH2O and evap. under a fan. Then scrape up crystals when dry. This is always done after acetone rinses to remove any remaining acetone so as to leave a totally solvent free clean product.

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#58 Myco-Iggy

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Posted 12 November 2007 - 12:59 PM

So right now swim got 2.4 of dreams from the 500 gram test.
But due to insufficient tools and glassware, probably could have
ended up with more.

Swim needs to acquire a hotplate, sep funnel, pipette, milligram scale and should get a distiller.

The hotplate and sep funnel are musts for this process though, and proper glass for boiling. Oh how swim wishes he had invested in proper flasks at first.

How ever one can improvise and produce some very very nice Xstals.
Twas swim's first true experience with mescal, and it was definantly swim's favorite.The body load was pretty heavy and probably thanks to tha ganj, swim didnt experience nausea but swim's friend had plenty.
Looking forward to many wonderful experiences.

As soon as swim can get some more money for equipment,
swim will finish the 1.5 kilos and go for some Re-Xstallizing.
Tried last night on the IPA/water but performed on only one gram.
Lack of proper equipment led to yet again another accident:mistrust:

Thanks again for all the knowledge, Ill report with my future attempts on cleaning.

PEACE
:rasta:

#59 tregar

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Posted 12 November 2007 - 02:29 PM

Thanks for the report Myco-Iggy.

I'll provide some pictures of how to do the re-crystallization with MEK (methyl ethyl ketone -- in the paint chemical isle) in the future perhaps.

I'll be turning off-white to tan to yellow mescaline into pure mescaline with photos of the "before" and "after" in dreams.

A distillation setup is not needed for any of this work, but a sep funnel, lab hotplate, a small erlenmeyer flask is, along with some sand, a cake plate, boiling stone. A buchner vacuum setup is good to have too to filter and rinse your crystals over when you pour the MEK through the buchner cup with round #101 to #103 filter disc.

I have had very light tan mescaline before at 300mg and less doses over a dozen times... it has no perceptable "body load" when nice & clean. Just euphoric and nice. There is no gas, no burping, etc. for the 1st 2 hour comeup either. It was so clean, I didn't even notice a "comeup". It is possible to get it clean...Yellow mescaline gives me gas and burping though for the 1st 2 hours. Brown mescaline caused nausea and weird body load for both of us, so we don't use it anymore. Very light tan to pure white or translucent mescaline is the bomb, though. Enjoyable as all get out, no bad body load. Purity does count for some sensitive people like myself & friend.

There should be zero nausea with 300mg doses and less of clean crystals, especially when 100mg dose is taken every 1/2 hour. I've never gotten even a hint of nausea when taking good clean crystals in 1/2 hour increments.

SWIM can always try an MEK re-crystallization if possible in the future in place of the iso/water re-crystallization...it gets the crystals really clean.

#60 tregar

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Posted 12 November 2007 - 02:32 PM

This is what a sand bath looks like on a lab hot plate, minus the flame source at the bottom--no flames allowed! ONLY a sparkless dedicated hot plate will do in a fumehood inside or outdoors. Also, an erlenmeyer flask should be used and not a beaker.

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