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Glass Shard Re-Crystallization Pictorial Options
 
Plasmod3smata
#1 Posted : 4/6/2008 11:34:30 PM

Justin Thyme


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Hello! This pictorial was created because of a lack of detailed information about the re-crystallization process. For some, like this kitty I know, learning about re-crystallization was frustrating as there were a lot of variations in method. Many were very similar and all had the same basic concepts but this pictorial is for anyone who has struggled with the process of transforming yellow or off-white powder into clear shards of DMT! Re-crystallization and be preformed multiple times however if one starts with yellow, off-white or white powder doing it one time can yield good clean crystals. Depending on how yellow your original product is a good amount of loss can be expected. A sacrifice for pure product! One that is very much worth it... smoking clear glass shards is as smooth as butter!

1. Obtain deep pot and fill it with hot water
2. Obtain strainer and set it in the pot of water and adjust level so the water comes up enough to cover half of a mason jar.
3. Turn heat on high to bring water to boil.
Note: Any other creative + safe means of a boiling waterbath will work for this, just make sure your holding container is not touching the bottom of the heating container.





4. Test digital scale accuracy using a 5g nickel (4.98, close enough)
5. Weigh out 1g DMT and put into a shotglass. Pyrex "mini-measure" shotglasses work well as they have ml markings on them.





6. Seal about 50-60ml of solvent (heptane works best) in a mason jar and let sit in boiling water bath for 15 minutes
Note: Unscrew lid and release pressure buildup as necessary. After 15 minutes solvent should have tiny sreams of bubbles in it but it may not.
7. Remove pot from heat.
8. Take jar of hot solvent, unscrew lid and swirl for about 10 seconds to let cool just a bit.
9. Pour about 25-30ml hot solvent into shotglass containing DMT. Typically a full shotglass worth.
10. Mix thoroughly with eyedropper.
Note: Stick eyedropper to the bottom of the shotglass and suck in + squeeze out solvent to thoroughly mix particles until all is dissolved.
11. Use eye dropper to fish out any hair\dust chunks that remain in the shotglass.





11. Remove strainer from pot and add ice cubes to reduce temperature.
12. Reduce temperature until a kitchen thermometer reads 150F
13. Put strainer back into pot and adjust water level so the shotglass can be placed on the strainer and the water will only come 3/4 up the glass.
14. Cover the shotglass containing the DMT solvent with foil and set into 150f waterbath.
15. Let sit for several hours until water is back to room temperature.





16. Remove shotglass from waterbath. Notice the separation of oils.
17. Use eye dropper to suck up yellow oils and squirt into second shotglass.
Note: In that new shotglass oil will sink and any DMT solvent you grabbed will float.
18. Tilt the second shotglass and suck back out any remaining clean DMT solvent and add back to original shotglass.
Note: As an alternative the clean solvent can be poured back into the original shotglass as the oil will stick to the bottom.





19. Take first shotglass with DMT solvent and pour into a third clean shotglass. The little bit of oil remaining will stick to the bottom of the glass.
Note: Notice in picture that once dried the remaining oil still contains a good ammount of DMT and should be saved for future re-crystallizing.




20. Cover shotglass with foil and let sit for 3-4 hours in room temperature then put in freezer for 24 hours.
21. After the freezer, pour off solvent into collection dish and put shotglass in front of a fan and wait 10-15 minutes or until dry.





22. Scrape crystals off and enjoy! Here are some pics, each one of a different batch, after only a SINGLE re-crystallization.



Razz
 

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Viracocha
#2 Posted : 4/7/2008 12:25:25 AM

..still lc..


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nice work mate Wink
what was the yield after recrystallisation?
 
XENONSION
#3 Posted : 4/7/2008 1:52:02 AM
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To grow your crystals large and in charge, i would not suggest freeze precipitating. Let your covered solvent sit at room temp for several days, then allow to evaporate slowly. This will give you the nice big crystal formations.

Just a variation you can employ, depending what you wanna do and how you want your final spice to look.

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danknugz81
#4 Posted : 4/7/2008 3:14:19 AM
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nice tek..

i've been cleaning via soda wash, melting the spice in a water bath, then allowing to cool back to room temp. dmt rocks! found the info on how to do this on the old board. easier to handle than the crystals for me. i dont mind the yellow personally. as long as there's no lye its clean enough for me.
 
Plasmod3smata
#5 Posted : 4/7/2008 3:40:13 AM

Justin Thyme


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Coschi wrote:
nice work mate Wink
what was the yield after recrystallisation?


White DMT usually had about a 10% loss... about 1g to .9g on one round and 500mg to about 430mg on another round.

Another batch went from 1g heavily yellow DMT to about 300mg clear glass shards.

Another batch had about 1.2g light-yellow DMT to about .8g of shards.

Another batch of 1.0g slight-yellow off-white DMT went down to about .8g bright white\clear shards.
 
Plasmod3smata
#6 Posted : 4/7/2008 3:40:24 AM

Justin Thyme


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XENONSION wrote:
To grow your crystals large and in charge, i would not suggest freeze precipitating. Let your covered solvent sit at room temp for several days, then allow to evaporate slowly. This will give you the nice big crystal formations.

Just a variation you can employ, depending what you wanna do and how you want your final spice to look.


Hmmm... do you use around 25-30ml per gram or more then that? I remember coAsTal growing large crystals by letting sit in a solution of around 50ml per gram...

It seems like in the super-saturated mixes a lot crystals form on the side of the glass within the first few hours of being in room temperature... so much so I didn't think leaving it for a few days would form large crystals... but it is something I definitely need to try!

Is it better to use closer to 30ml per gram or closer to 60ml for the slow-evaporation during large crystal formation?
 
XENONSION
#7 Posted : 4/7/2008 4:03:23 AM
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Plasmod3smata wrote:
XENONSION wrote:
To grow your crystals large and in charge, i would not suggest freeze precipitating. Let your covered solvent sit at room temp for several days, then allow to evaporate slowly. This will give you the nice big crystal formations.

Just a variation you can employ, depending what you wanna do and how you want your final spice to look.


Hmmm... do you use around 25-30ml per gram or more then that? I remember coAsTal growing large crystals by letting sit in a solution of around 50ml per gram...

It seems like in the super-saturated mixes a lot crystals form on the side of the glass within the first few hours of being in room temperature... so much so I didn't think leaving it for a few days would form large crystals... but it is something I definitely need to try!

Is it better to use closer to 30ml per gram or closer to 60ml for the slow-evaporation during large crystal formation?

I heat my solvent, and use a small shallow glass dish instead of a shot glass (easier to scrape out). I only add enough solvent to dissolve the dmt, no more then JUST enough.It is not much at all, nowhere near a shot glass full for sure. Then just cover and let it sit and grow.

This is my glass i use for growing crystals


And here are some of what i've grown. Once i notice it stops growing, i uncover and let it evap. You can get half a gram into one large crystal clump, it's pretty neat really.










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DrParadox
#8 Posted : 4/7/2008 4:24:29 AM
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Nice.

The last one looks like a maple leaf!
 
Plasmod3smata
#9 Posted : 4/7/2008 4:58:40 AM

Justin Thyme


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Sweet deal! Seems easy and effective!

Will try that tomorrow and see what comes up over the next few days!

You can't beat big crystals of awesomeness!
 
danknugz81
#10 Posted : 4/7/2008 5:14:06 AM
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those crystals looks awesome xeno.. gotta try that next time
 
XENONSION
#11 Posted : 4/7/2008 5:38:14 AM
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DrParadox wrote:
Nice.

The last one looks like a maple leaf!
haha, yea that last one was huge too. like half an inch maybe across. it was all once big piece. I felt bad breaking it up and smoking it, haha.

but like i said, it's all relative to what you want as a final product. a nice pile of pure white, or some big crystals. both are nice to have. I did notice the big crystals melted easier at warm temps.(90F and up) So take that into consideration.

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danknugz81
#12 Posted : 4/7/2008 7:10:01 AM
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how many days did those take to form?
 
Viracocha
#13 Posted : 4/7/2008 9:35:05 AM

..still lc..


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nice crystals XENO!
love those crystals Very happy Very happy Very happy
whenever I hand out crystal it's crystal, not fluff Wink
 
XENONSION
#14 Posted : 4/7/2008 3:50:25 PM
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danknugz81 wrote:
how many days did those take to form?
the first photo..those were only after sitting overnight. total i usually let it sit about 2-3 days.

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Spock's Brain
#15 Posted : 4/7/2008 5:58:12 PM

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maybe you could sell the maple leaf crystal to a collector on e-bay for $1300, simalar to the illinois shaped corn-flake that had been in the news recently!!!

http://timesofindia.indi...articleshow/2889010.cms
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kagenical
#16 Posted : 4/7/2008 9:55:49 PM
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I wonder how quickly that eBay auction would get shut down. Razz.
 
habib
#17 Posted : 6/27/2008 6:44:00 PM

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Plasmod3smata,

thanks for posting this pictorial. Sal just tried your process for the first time, he had been having a little difficulty with this. In the process, he did discover what he thinks is the main problem with many re-x tutorials, and that is: depending on the purity of one's extractions, 1 gram of yellowish/off white powder may be too much for one shot glass. In his experience, one shot glass could not hold enough heptane to dissolve the whole gram. When Sal read XENONSION say : "You can get half a gram into one large crystal clump, it's pretty neat really." he realized he should probably be working with less than a gram per shot glass/container.

He tested his theory and it worked thus far. Perhaps it is because his spice is less pure, although he is doing STB with carbonate washes, so he cant imagine his is that different. He would advise working with .5g or maybe .75g rather than 1.

Thanks for the hard work and awesome pics.
H
 
69ron
#18 Posted : 6/27/2008 8:43:43 PM

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XENONSION wrote:




The yellow discoloring is most likely DMT n-oxide. This is the main problem with growing the crystals slowly when exposed to oxygen in the air.

Growing Large Cyrstals Without Forming DMT N-Oxide


What you do is you have two containers, one that fits inside the other. You put a little zinc dust on the bottom of the larger container to absorb oxygen, and you put anhydrous magnesium sulfate to absorb any moisture build up. Or even better, use a tiny canning mason jar. You put your freeze precipitation solvent mix in a smaller container that fits inside the larger container. You place that on top of the zinc dust and magnesium sulfate, and then you close the lid of the larger container so that it’s air tight. Both containers should be Pyrex glass and the lid must be freezer safe and flexible enough to account for the pressure changes cause by the change in temperature.

Once in the container you do one of the following methods.

Cheap Kitchen Method

You let it sit for 2 days at room temperature. Then 2 days in the refrigerator. Then 2 days in the freezer. This produces an effect similar to slow evaporation except that there is no fresh oxygen or moisture present to degrade the DMT because the lid is closed and you have zinc dust and anhydrous magnesium sulfate taking care of what was in the container when the lid was closed. When you’re done you open the container, take out your DMT container, pour off the haptane and dry the crystals in a vacuum or open air at room temperature (without a fan!).

Lab Method

What works even better is to put the closed container on a digital hotplate that can reduce it’s hotplate surface temperature. These are available but cost quite a lot. This is done like above except it’s kept on the hotplate most of the time. You start by putting the container on a hotplate set to 40 C. Everyday you reduce the temperature by 10 C. On the 5th day you are at 0 C (or 5 C, because many hotplates only go down to 5 C). On day 6 you place it in the freezer set at the coldest setting (usually -15 C or below). When you’re done you open the container, take out your DMT container, pour off the haptane and dry the crystals in a vacuum or open air at room temperature (without a fan!).

Long Term Storage

Place the DMT inside a small glass container that has a screw on cap with whole drilled into it. Put a good quality flexible glass micro fiber filter paper on top of the container and close the lid so that the filter paper is held firmly in place by the lid. This filter is there to prevent dust from getting inside the container while allowing the oxygen in the container to flow out of the container. In a larger container place a small amount of zinc dust and anhydrous magnesium sulfate just like before. Place your DMT container in the larger container. Close the lid of the larger container using a flexible air tight lid that is freezer safe. Because the DMT is protected by a filter paper, if the larger container is ever accidentally shaken, the DMT will not get contaminated with the powder in the larger container. Also, the filter paper allows the zinc dust to absorb all the oxygen present in the DMT container.

Manufacturers and sellers (such as Sigma-Aldrich) recommended that 5-MeO-DMT be stored at 2 - 8 C and NOT KEPT FROZEN. So this probably applies to DMT as well. Actually this applies to the majority of drugs. It might be a good idea to buy a small freezer adjusted to 5 C just for this purpose.
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Faust
#19 Posted : 11/7/2008 6:57:52 PM

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Excellent thread, great pictures, might not be the right method for someone who's crystals are not relatively clean already.

Great info on DMT N-Oxide, 69ron. As it relates to re-xtallyzation.

Getting clear spice from something like Vovin's Tek and then re-xtallizing with this Tek would be ideal, I think.
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acolon_5
#20 Posted : 11/7/2008 8:46:31 PM

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I only want to note that to increase your crystal size even further one should remove the cover on the recrystalization container after growth stops. Let it evaporate until there is only a very small amount of heptane left in the container....your crystals will grow even larger.

The remaining heptane can be used to recrystalize the yellow goo, or added to the next freeze precipitation.

I have found that I can partially cover the container slowing down the evaporation rate, or I can add a % of naphtha (after the impure dmt has been disolved in heptane and moved to a new container) to slow down evaporation. Both of these methods will grow wonderfuly large crystals, just make sure there are no vibrations where the container is going to sit, the less vibrations the larger the xtal.

Also, I want to note that I have not observed much discoloration when leaving the containter out in the open unless I sit it in a warm place. I almost always come out with very nice clear crystals. In the pics above you can see the yellow is mostly at the bottom.

I have noticed that bestine does pick up a small amount of oils (hotter bestine = more oils dissolved) and those will crash out before the DMT does. To avoid this I will use a little more bestine than needed and not heat it up as much. I will then dissolve my spice, and let it sit for a few minutes (4-5 at most). Most of the oils will fall to the bottom and can be sucked out or the solvent can be moved to a new container. The resulting spice has almost no yellow coloration.
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