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DMT STB Extraction.... Need help with Recrystallization Please !!! Options
 
mimosadmtastronaut
#1 Posted : 10/14/2010 6:31:55 PM
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Hey Everyone! SWIM is in the process of finishing up his first DMT extraction. The method he used was a Straight to Base Tek done by Whatchamacallit that was posted on a different forum. SWIM basically followed Whatchamacallits STB Tek to the letter.

just in case... Ill post the PDF for the Tek as well Smile

SWIM started with 500g MHRB . Added the lye to H20, proceeded to add the MHRB , then did each pull with 400ml Naptha and completed five total pulls. Then SWIM did the soduim carbonate wash twice and then the cold tap water wash very quickly in order not to ionize the DMT and to get rid of any remaining lye/carbonate. He then added the cooked Epsom salts, filtered that through a 2liter and coffee filter. THEN is when SWIM noticed some residual dark orange matter near the bottom. SWIM used the sep funnel to get that out and proceeded to freeze for 50hrs. Decanted the Naptha , collected the ingredients on a pyrex glass dish and let evap for a few hours. What came out is what was seen in the pics, large chunks on fairly dark orange spice.....

*From 500g MHRB SWIM ended up with a yield of just over 6.4 (6.401g) grams of medium dark orange DMT , with many many big crystals and some powdery bits as well. SWIM plans to try out a small batch tonight of the orange DMT yet thinks he may now need to run a re-crystallization to purify a little bit and get some lighter colors. He thinks the dark color may result from a new vendor providing the MHRB or possibly the polar wash wasnt done perfectly. Hence the need to do one more quick filtration before popping the jug into the freezer.


Can anyone give SWIM some advice on a proper and effect recrystallization process? (ive gone through tons of threads yet am i still just a bit concerned to try it out.....

Also, could anyone have any other thoughts on why the dark color? SWIM shall provide pics very soon..... :-D sorry if they come out sideways.... also, SWIM am still drying them off because he caught a very very slight whiff of solvent still, so SWIM thinks he shall chop the yield up a little bit to properly and thoroughly dry out all the DMT , yes/no?



 

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gammagore
#2 Posted : 10/14/2010 11:16:31 PM

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Should I wash my spice?

How to re-x

The FAQ is your friend use itSmile

When drying the freebase I always chop it up nice and good, and chop till no more smell of solvent is present. This way you get out any trapped solvent.

The color that is in the spice is just some tannins and oils/fats. These tend to be quite present in STB extractions. From the pics you provided it looks like your spice just needs a bit of cleaning. Try a few re-x's.
 
mimosadmtastronaut
#3 Posted : 10/15/2010 2:14:04 PM
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Thanks Gamma! Yeah SWIM has been on the site for a long time but finally needed some help myself. SWIM actually did read through those and many many many others on various forums. but thanks for the links, he will take another look. SWIM really wanted to get the pics up of his first extraction and because of the nature of the yield.

SWIM was curious on the overall return on his product. 500g of MHRB from a new "sponsor" and a yield of 6.401g. And then, looking at the color of the dmt; SWIM thinks there would be significant loss due to impurities so SWIM is estimating to return ~4G after Re-Xing probably. SWIM was having a lot of trouble locating Heptane/Bestine in the Midwest though. After several trips to art supply stores/hardware locations, he is still without his solvent. He does still have naptha laying around from this extraction, yet the top of the can has had a tiny hole in it because the can was unable to be opened for the initial extraction. it also has been stored outside on SWIM's balcony covered and slightly protected. does anyone think this could still be used or is it best to just get a new bottle of naptha/bestine (if located)?
 
gibran2
#4 Posted : 10/15/2010 2:54:23 PM

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When a product is that impure, it might be easier to do a “mini” A/B if you want really white crystals.

It’s simple:

---- Dissolve product in a small amount of vinegar – just enough to dissolve all of it.
---- Dilute with water (maybe 500mL or so?)
---- Prepare a small quantity of NaOH solution (about 5g NaOH in 100mL water)
---- Add NaOH solution to DMT solution. Freebase will immediately precipitate.
---- Extract as usual.
gibran2 is a fictional character. Any resemblance to anyone living or dead is purely coincidental.
 
mimosadmtastronaut
#5 Posted : 10/15/2010 3:40:08 PM
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Ohhh, that's an interesting idea.... SWIM was going to try to obtain some Bestine today and begin a re-X tonight. From what SWIM has read, one would need to first heat up some Bestine. Now, SWIM is a little concerned about using such flammable materials within close range of a stove so he was thinking to use a Candle Warmer. Now - wax has a melting point of 125 degrees F. This seems like the perfect temp to get the solvent warm.


**SWIM was hoping to heat the solvent on the candle warmer, using a glass mason jar and get it to approx ~125*F,
(Or possibly use the candle warmer to heat water in a mason jar and then place the solvent in a smaller jar and place that in the water?)

**He would then saturate the DMT in a shot glass or small glass container
[would a small glass flip top airtight container work? - look at picture]

**Wait for the impurities to settle at the bottom

**Then either, remove the solvent/dmt and place into a new container or siphon out the junk on the bottom and transfer?

**Next, this could either be: [1] freeze precipitated overnight
[2] cover and get the crystal grow, once they stop, uncover and evap (Which i am thinking maybe the best way!) ???


or..... Start from the beginning and:

Saturate the Spice with Bestine and apply around a 130sh degree bath to it. It should not take long to disolve completly. Then put it in a cooler over night to slowly cool it down making the seperation of the jungle alkoids very easy. The next day take it from the room temp cooler and cool it in the fridge till it hits 50sh degrees, You can tell cus the top layer will be fairly clear, and the bottom will be filled with gunkie material. Pour of the solvent leaving the nasty at the bottom in there as you can pull it out later if you want some jungle goo. Take the newly aquired goodies in solvent and freeze precip again. After freeze precip you should see some very nice whiteness to it that wasn't there before if your load was that dark. Take that freez precip and pour off the solvent from the spice.. but leave a little bit of the solvent in there with it. Enough to redisolve the goodies. So now you have a jar with a fairly good amount of much cleaner Spice with some bestine still in it. Back to the water bath. 130sh degrees. Redisolve the goodies in the very small amount of bestine, and remove it from the heat. If done right it should cloud up quickly as it cools and the crystals try to drop out. Thats a good thing. Quickly pour off the cloudy bestine on a pyrex dish. Let this evap slowly with no direct wind on it. Like a cabinet or closet .. whatever. You should have great crystal formation as it cools down and evaps. The will bunch up in like flower shaped chunks or shards of beauty.



What do you guys think???
mimosadmtastronaut attached the following image(s):
jar.jpg (4kb) downloaded 233 time(s).
 
justine
#6 Posted : 10/15/2010 4:01:58 PM

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Well, if you put your saturated solvent in the fridge dmt will obviously precipitate and mix with the oil/lye/n-oxide/...
I usually sodium wash my solvent before freeze precipitation but I didn't do it for my last stb pull and I only needed two
evap re-x to convert orange/red dmt goo to perfectly white crystals. I just did it like advised in vovin's tek (pour hot solvent, swirl, let
the goo settle, pour).
To see the world in a grain of sand, and to see heaven in a wild flower, hold infinity in the palm of your hands, and eternity in an hour.
- William Blake
 
ucorky
#7 Posted : 10/15/2010 4:09:19 PM
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well, open flame is a big NO NO. My dear Uncle Swimmie here reliquified some just by running hot water on the side of his beaker that he uses and swished it around. He's too new to this but does know NO OPEN FLAME is tolerable. NONE. Its all done in different rooms and buildings in his case. A drying house if you will. lol. Pardon me if I sound stupid, because I am. Smile
Any references to ingested drugs or substances are understood to be legally obtained, grown, or prescribed or may not exist at all. Ucorky is the name of a character in an upcoming book on ficticious dreamers. Any references of the above or by SWIM, SWAM, SWARM, Uncle Swimmie or SWIMICTIN are purely a matter of conjecture. To, TOO and TWO =2
 
mimosadmtastronaut
#8 Posted : 10/15/2010 4:21:16 PM
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justine wrote:
Well, if you put your saturated solvent in the fridge dmt will obviously precipitate and mix with the oil/lye/n-oxide/...
I usually sodium wash my solvent before freeze precipitation but I didn't do it for my last stb pull and I only needed two
evap re-x to convert orange/red dmt goo to perfectly white crystals. I just did it like advised in vovin's tek (pour hot solvent, swirl, let
the goo settle, pour).


Yes, the DMT would def start to precip out and we wouldnt want that.
When i did the STB, i did two sodium carbonate washes and then the quick h20 wash.
As you can see by the pics, the DMT did come out to a dark orange color.

Would you happen to have a link to Vovin's tek by chance?


So I should heat the bestine/ pour that into say a glass mason jar/ swirl and sit to let the impurities settle/ then extract that to a new container and then evap until crystals form?
 
justine
#9 Posted : 10/15/2010 4:53:26 PM

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mimosadmtastronaut wrote:
justine wrote:
Well, if you put your saturated solvent in the fridge dmt will obviously precipitate and mix with the oil/lye/n-oxide/...
I usually sodium wash my solvent before freeze precipitation but I didn't do it for my last stb pull and I only needed two
evap re-x to convert orange/red dmt goo to perfectly white crystals. I just did it like advised in vovin's tek (pour hot solvent, swirl, let
the goo settle, pour).


Yes, the DMT would def start to precip out and we wouldnt want that.
When i did the STB, i did two sodium carbonate washes and then the quick h20 wash.
As you can see by the pics, the DMT did come out to a dark orange color.

Would you happen to have a link to Vovin's tek by chance?


So I should heat the bestine/ pour that into say a glass mason jar/ swirl and sit to let the impurities settle/ then extract that to a new container and then evap until crystals form?


https://wiki.dmt-nexus.m...tek#Step_9:_Solvent_Wash

Well that's how I do it but I certainly do not pretend it's the best way, it just works great for me.

And by the way, I once had a batch of slightly orange dmt and it was the most powerful I ever made, it even tasted great (some kind of... spicy... after-taste, hard to define but
really incredible).
To see the world in a grain of sand, and to see heaven in a wild flower, hold infinity in the palm of your hands, and eternity in an hour.
- William Blake
 
mimosadmtastronaut
#10 Posted : 10/15/2010 5:59:16 PM
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Cool, thanks for the link. I ended up downloading the PDF and taking a look. That seems like it would be a proper tek to follow. SWIM is just wondering how long the evap would take? also, would it be possible to take the dmt/solvent solution and freeze precip that to possibly speed up the process?

 
justine
#11 Posted : 10/15/2010 6:08:56 PM

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In my case it takes around 24h to fully evap 50ml of naphta in a 10cm wide plate at room temp with the windows open. Freeze precip is also possible but I like to get nice crystals Smile
To see the world in a grain of sand, and to see heaven in a wild flower, hold infinity in the palm of your hands, and eternity in an hour.
- William Blake
 
mimosadmtastronaut
#12 Posted : 10/15/2010 6:34:15 PM
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Let me ask, you are using naptha for the recrystallization. From what ive read, apparently Bestine (Heptane) would be the best solvent to use in the re-x.

I currently have a large amount of naptha laying around from this extraction on monday. The problem was, the top of the can was impossible to open and so a small hole was placed in the top. This was covered with a blanket and basically sat outside on my balcony for the past 4 days. Would this deteriorate the quality of the naptha? would it still be usable for the recrystallization?

I was trying to obtain Heptane but it has become quite difficult to find in the midwest. I was actually going to try one more place tonight and if acquired, should i use that or just the said naptha?
 
justine
#13 Posted : 10/15/2010 6:45:27 PM

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mimosadmtastronaut wrote:
Let me ask, you are using naptha for the recrystallization. From what ive read, apparently Bestine (Heptane) would be the best solvent to use in the re-x.

I currently have a large amount of naptha laying around from this extraction on monday. The problem was, the top of the can was impossible to open and so a small hole was placed in the top. This was covered with a blanket and basically sat outside on my balcony for the past 4 days. Would this deteriorate the quality of the naptha? would it still be usable for the recrystallization?

I was trying to obtain Heptane but it has become quite difficult to find in the midwest. I was actually going to try one more place tonight and if acquired, should i use that or just the said naptha?


The wiki states that heptane and naphta share a similar xlogp, which means they should both dissolve molecules in the same way so as far as re-x is concerned you can use any of the two interchangeably.

I think your naphta shouldn't have picked up moisture but even if that's the case it will only take longer to evaporate.
To see the world in a grain of sand, and to see heaven in a wild flower, hold infinity in the palm of your hands, and eternity in an hour.
- William Blake
 
mimosadmtastronaut
#14 Posted : 10/15/2010 8:21:18 PM
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Great! SWIM was hoping to use that Naphtha for my next extraction as well!
As for the re-x, SWIM located a art supply chain who carries the 4oz small bottles of Bestine so he shall be attempting the three shot glass method tonight... and i shall post up some pictures tomorrow or whenever the drying is complete Smile

Thanks for all the help so far Smile

 
mimosadmtastronaut
#15 Posted : 10/16/2010 7:11:11 AM
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So SWIM got a hold of some Bestine this afternoon. He went about the three shot glass method of re-x-ing. He made a heat bath, warmed the bestine in one glass, put crushed dmt in the second. Then took an eye dropper to transfer the warm bestine to the dmt. Then let it dissolve, removed the bestine with the dropper into a clean new glass. Threw that into the ridge for 45 min and then into the freezer. Within 30 min SWIM could see many crystals beginning to form. After being in the freezer for just over 3 hours, SWIM could see many many beautiful tiny crystal clear flower like petals sprouting in the bottom of the shot glass. Tomorrow i will add some pics of the process/reward to let you guys know how it went and maybe get your opinion Smile SWIM has to say, this was a suuuuuper easy method which seems, at least in the early stages, to be a great clean up to produce some beautiful crystals.....


SWIMs question would be, how long should they ideally stay in the freezer? 24 hrs? ...or would something like 10-12 work as well?

Also- how would one go about creating larger crystals?

I currently have a first experiment of .200mg dmt going with approx 25ml of bestine going as well as the second experiment of .300mg dmt with approx 15ml bestine.

Could i ideally take one of those, do the evap, then begin another re-x and instead of adding that to a new shot glass, could i add it to one of the existing 1st/2nd shot glasses that i was already working with? Could this possibly cause crystal to grow on top of existing crystals- similar to doing a real lab setting recrystallization where one would save one crystal and place it in the container to initiate growth? just a random idea- doubt it would work but was just curious on the matter lol


 
 
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