
Re-crystallization of mescaline hcl attempt w/photos
#1
Posted 05 February 2008 - 04:38 PM
#3
Posted 05 February 2008 - 04:39 PM
#4
Posted 05 February 2008 - 04:40 PM
#6
Posted 05 February 2008 - 04:41 PM
Materials used next: 125 to 150 mL erlenmeyer flask, funnel, stir magnet.
As you can see the "drying" of the MEK worked well, the resulting MEK is free of epsom salt particles and looks crystal clear.
#7
Posted 05 February 2008 - 04:42 PM
The 150 mL of dry MEK is hooked to a buret clamp ($4.95).
The buret clamp is hooked to a ring stand.
The flask holding the MEK is suspended about an inch or so above the bottom of a stainless steel mixing bowl.
#8
Posted 05 February 2008 - 04:43 PM
#10
Posted 05 February 2008 - 04:47 PM
Also, persona let me know that if I'm using a stir bar, I don't need to add stones. Thanks persona!
The mescaline hcl was previously collected by gassing and collection from a sep funnel with water. So it's shade is somewhere between beige and yellow. This stuff is really powerful and gave us a really great trip at only 200mg for both people, resulting in a laughing fit for hours, watching comedic movies was very entertaining and was tons of fun. The last time we had a trip that good was when we took a couple hits of acid each. However, for the comeup during the 1st 2 hours, we got some gas and burping resulting from the impurities in the yellowish looking mescaline (collection 3rd or 4rth pull with hot water in sep funnel). The impurities need to be taken out so there will be little to no discomfort during the comeup.
In the future, when I gas, I will collect directly with filters instead of sep funnel and boiling hot water. This gets some pretty nice looking clean stuff.
We will break out the fume hood tomorrow, add the 3 grams of mescaline hcl to the flask, get the water bath boiling and see where it goes from there, wish me luck.
1) From what I've read, I think at first the MEK will appear cloudy from the undissolved mescaline in the MEK, then I will add drops of water until the MEK turns clear....(meaning all the mescaline has dissolved into the solution)...then we will boil it down till it starts to have a "shimmy look", that's when we take out of the heat and put the flask in the freezer to see if any crystals form after a few hours....if not we put the flask back in the hotplate bowl of water and boil it down further.
2) Alternately, I could just take the flask out of the mixing bowl when it starts to "shimmy" and let it cool down to room temp, then put it in the fridge, then move it to the freezer...this should result in even larger purified cystals.
I'm not sure which route to go for a first attempt. Opinions are welcome.
Attachments:
#11
Posted 05 February 2008 - 04:48 PM
I mean the process and all is very easy, and no there was not any explosions or glass breaking or anything like that, I just mean, it's hard to tell when to stop adding water droplets (I stopped at 80 drops) due to the yellowish/orange color of the mek once all the mescaline has been added and it's been boiling...anyhow here's what happened:
It's hard to tell when you have reached the "clear" looking stage after adding water dropplets when your MEK is discolored yellow/orange...but I did get it to go from cloudy to somwhat clear with 80 water drops...maybe this is too much, maybe not enough, hell I don't know.
Materials set up inside the homemade fume hood with 6 Radio Shack fans, the fumehood was backed up to an open back window with a light curtain on it...it helps alot, because once you hit 180 degrees F, you can smell the ketone, like me! once mentioned some people like the smell of boiling ketones and others don't, I dont seem to mind it. It's not that bad, but you will want a powerful fume hood running to draw the fumes out.
Those are the safety goggles to the left, and to the right is a glass of distilled water and dropper. I kept a fire extinguisher nearby on the floor, and tried it out just to make sure it worked by pulling the pin and squeezing the lever, had it on standby just in case...but I'm happy to report that all wen't well, and now that I've done this, even if it turns out to not be successful this first time, that at least I'm not scared anymore to do this...I didn't shit my pants or catch on fire or anything like that so I'm more than happy. It was a piece of cake.
That's a clip on thermometer so I could read the temperature during the process...at 180 degrees is when the MEK starts to boil off. The water bath never got over 195 degrees or so, so I must say no matter where you set the "temp" rheostat/potentiometer setting on the hotplate, you will be able to keep a perfect water bath temp. It will always be 212 degress or less..this is perfect for this process. I kept the potentiometer at the "1" or "2" setting for most of this, except when I first started the water boiling, I cranked it up to "6" or so to get the water nice and hot really fast. All of this takes time to get the water up and boiling so make sure you have an hour or two set aside.
#13
Posted 05 February 2008 - 04:49 PM
Not easy to determine the correct amount of drops! But this was my first time...
Then I let it boil down all the way till about the 85mL line on the flask, that's when I noticed a "ring" of tiny crystals forming around the inside of the flask at that level. Your "supposed" to boil down from "clear looking" to "shimmery looking" and stop the process, that's when you take it off the heat and let crystals form, but once again this was hard to determine as I could not detect a "shimmy" looking solution due to the discolored MEK. So I went by when I could see a ring of "tiny crystals" forming around the inside, when I started to see them forming, that's when I stopped the process, and took it off the heat and transferred it to the freezer...I am transferring to the freezer instead of letting it go from hot to room temp, to fridge, to freezer, because I just wanna see if I'm gonna get anything, this being my first time...next time I'll go out and let the crytals form big by slowly letting the temp drop over time.
#14
Posted 05 February 2008 - 04:50 PM
This is after the spinning stopped, the mescaline has fallen out and collected at the bottom, I could tell, because when I lowered it back in the hot water bath and started the spinning again, a pool of white looking mescaline spun off the bottom of the flask and went spinning back into the mek & water solution.
#15
Posted 05 February 2008 - 04:50 PM
You really can't see the tiny crystals very well with this photo, but I could see them forming.
#16
Posted 05 February 2008 - 04:51 PM
If not, then it's back to the lab again on another day when I've got some free time.
Here it is one hour later, I shined a high powered LED flashlight on the flask in the freezer and it has a thick layer of fluffy looking white crytals forming all over the place (but pic does not show it very well) so this is very promising! :headbang:
I'll wait a day (till tomorrow night) then go ahead and filter off the purified crystals.
#17
Posted 05 February 2008 - 11:06 PM
And the end result = .6 gram of perfect white mescaline, this stuff is exactly like talcum powder ! It is fine, fine, fine, you can even "rub" it into your skin and it will disappear it is that fine.
I have never seen anything like it !!!
This is the stuff that "crashed out of the MEK" in the freezer--it was floating around in the top to middle to bottom layer of the MEK.
I am going to take the stuff at the bottom of the flask and re-crystallize it again, this is the stuff that fell out super-early while it was boiling in the MEK and WATER mix because I used TOO MANY WATER DROPLETS, I should have used more like 10 drops, and not 80 drops !!!
Had I used a much lower amount of water drops, I would have had a much greater return of crystals crashing out of the MEK in the freezer.
This picture was taken WITH NO FLASH, it really does appear this white, just like snow.
I am amazed beyond belief--perfectly snow white mescaline hcl !!!
Next time, I will get the water droplet ratio right so I can get a much greater return of all perfect white.
#18
Posted 05 February 2008 - 11:25 PM
It is not AS perfectly white as the .6 gram that crashed out in the freezer, but it's pretty damn close.
Again, it is also just like talcum powder, and if you rub a pinch of it on your skin, it will disappear into it.
It is fine, fine, fine.
#20
Posted 05 February 2008 - 11:53 PM
I love the use of a foodsaver, it's so elegant and awesome. Any idea how many mmHg it'll pull? Does it struggle? Have you used it for any length of time, or just for vacuum filtration? Haha, sorry to go off-topic in the first reply, but I've been shopping around for a replacement for my aspirator setup.
Great job man.