Re-crystallization of mescaline hcl attempt w/photos
Started By
tregar
, Feb 05 2008 04:38 PM
103 replies to this topic
#1
tregar
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Posted 05 February 2008 - 04:38 PM
This will be posted over two days.
#2
tregar
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Posted 05 February 2008 - 04:39 PM
Materials: 1 quart MEK, 1 liter jar, 2 handfulls of dried epsom salts (were dried in oven at 400 degrees for 2 hours then scraped off baking pan with a spatula)
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#3
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Posted 05 February 2008 - 04:39 PM
MEK is poured into the jar with 2 handfulls of dried epsom salts and allowed to sit for 1 hour...every 10 minutes or so the jar is shaken. The dried epsom salts will serve to pull the water out of the MEK rendering it dry, which is what we need for the re-crystallization.
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#4
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Posted 05 February 2008 - 04:40 PM
1 hour later....now it's time to pour the MEK off into a buchner vacuum flask with a #103 filter disc. The deluxe foodsaver is used to generate the powerful vacuum pull...this has never failed me, a great vacuum source. The tubing is mated to the line from the foodsaver using plumber's tape.
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#5
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Posted 05 February 2008 - 04:41 PM
The MEK after it has filtered thru the #103 filter disc...it filtered rather quickly...took only 2 minutes.
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#6
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Posted 05 February 2008 - 04:41 PM
The dry MEK from the buchner flask is then poured off into a vacant clean jar.
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.
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.
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#7
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Posted 05 February 2008 - 04:42 PM
Materials: hotplate with stirrer, ring stand, buret clamp, stir magnet, steel mixing bowl filled with water (to the level of the MEK or slightly below the MEK level) that will be heated by the hotplate.
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.
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.
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#9
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Posted 05 February 2008 - 04:46 PM
Closeup view of the flask suspended in the mixing bowl, water has not been added to the bowl yet, will continue tomorrow.
Stir magnet has been added to the flask with MEK.
Picture below.
Stir magnet has been added to the flask with MEK.
Picture below.
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#10
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Posted 05 February 2008 - 04:47 PM
Approximately 3 grams of mescaline (2.94 grams) was weighed out and will be added to the 150 mL boiling MEK in the flask. Some boiling stones will be added to the flask and stirring will be commenced. This will serve to prevent "bumping" as well as quickly dissolve the drop(s) of water into the MEK. I will stop the stirring whenever I need to get a good look at the condition of the solution (ie...cloudy, clear, shimmery) so I will know how to proceed. After each drop of water I will stop the stirring to observe the visual condition of the solution. This is more an art then a science from what I've read from others.
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.
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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.
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#11
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Posted 05 February 2008 - 04:48 PM
Damn, this has not been easy! I've got the mixture chilling in the freezer now, it has a visible layer of white mescaline at the bottom that appeared to fall out before even placing it in the freezer, I noticed a ring of tiny "crystals" forming around the 85ml line so I stopped the boiling ketone and transferred it to the freezer.
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.
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.
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#12
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Posted 05 February 2008 - 04:49 PM
Here we are starting out with 3 grams mescaline, 125 ml of dry MEK, and 100 degrees and climbing on the thermometer. There is water in the water bath, I added more later to get it to where it was about 1/2" to 3/4" below the level of the MEK.
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#13
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Posted 05 February 2008 - 04:49 PM
Here we are at around 188 degrees F, once I hit 180 degrees F, you could smell and see the MEK boiling away, that's when I added about 80 water droplets, till I noticed it turn from "cloudy" to "clear", although I must admit this was extremely difficult, and the hardest part of the process, because my MEK solution was allready discolored yellow/orange/light brownish from the dissolved impurities.
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.
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.
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#14
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Posted 05 February 2008 - 04:50 PM
Here's what I'm talking about, see the pic below, I pulled the solution out of the heat to show you how discolored it is, that's why I'm having a hard time determining "cloudy" from "clear" from "shimmery". Talk about impurities!!!
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.
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.
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Posted 05 February 2008 - 04:50 PM
I pulled the flask out of the heat (when the MEK & water boiled down to about the 85mL level) when I started to see a ring of tiny crystals form around the inside of the flask at the MEK top level.
You really can't see the tiny crystals very well with this photo, but I could see them forming.
You really can't see the tiny crystals very well with this photo, but I could see them forming.
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#16
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Posted 05 February 2008 - 04:51 PM
The flask is now in the freezer sitting undisturbed...so I'll check to see if I got any purified crystals later on.
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.
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.
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#17
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Posted 05 February 2008 - 11:06 PM
I couldn't wait, so I took it out of the freezer 8 hours later.
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.
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.
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#18
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Posted 05 February 2008 - 11:25 PM
And here's the rest of the mescaline that was found resting at the bottom of the flask--as you can see it has been cleaned or purified free of any yellow or orange or brown impurities...
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.
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.
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#19
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Posted 05 February 2008 - 11:40 PM
Look at all the orange/yellow/brown tinted impurity crap that the MEK removed from the mescaline hcl !
Amazing isn't it ? Remember, we started with CRYSTAL CLEAR MEK.
Amazing isn't it ? Remember, we started with CRYSTAL CLEAR MEK.
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#20
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Posted 05 February 2008 - 11:53 PM
Wonderful writeup and great pics!
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.
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.
