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Slightly orange DMT that sinks to the bottom when crystalizing Options
 
DmnStr8
#1 Posted : 2/25/2018 5:37:30 AM

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Nice crystals there!

No advice as far as color goes. Perhaps its just tannins? Dunno..

Maybe try Rx again... maybe that would provide a whiter appearance each Rx. I have done multiple Rx and got whiter and whiter crystals.

"In the universe there is an immeasurable, indescribable force which shamans call intent, and absolutely everything that exists in the entire cosmos is attached to intent by a connecting link." ~Carlos Castaneda
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
concombres
#2 Posted : 2/25/2018 6:35:08 AM

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I do my recrystallizations a little differently than what i typically see described here but it works well to separate white DMT out.

what i do is throw all my DMT in a shotglass with 10ml of heptane. Warm with a hot watwr bath until i see the dmt melt & go liquid, swirl & let it dissolve for another two or three minutes, then pour the heptane off into a separate container.

From there usually the gooier yellow stuff stays in the original shotglass & i will pul from that a few more times with fresh heptane. The yellow usually seems to get darker the more white DMT i pull from it.

It requires a little skill because too much solvent, too much heat, or both will dissolve a little of the yellow. There is s balance between solvent volume per pull & heat but i usually just do things by eye.

From there you should be able to use the white DMT to grow a few seed crystals & use those to start growing larger clusters. Heptane is better for purification than growing large crystal. You want something that holds onto DMT a little better as the temperature drops to allow for crystal formations to form slower & grow large rather than quickly crashing out & forming needle clusters.
 
tydel24
#3 Posted : 3/6/2018 12:31:04 PM

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afer i got a few clean looking pulls of my enriched solvent,, i found letting it just sit in front of a fan before freezing can crash out a lotta the goo, an hour 2 tops, then you can pour away from said gooey dish to a clean one, you should find a layer of gooey brown fats and oils on it,, mightbe hard tosee til you start scraping. then freeze,, GOOD LUCK!
 
tydel24
#4 Posted : 3/6/2018 12:34:03 PM

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2headsARE1 wrote:
I'm in the middle of a recrystallizing project, aiming to get large crystals. I have some DMT that has been purified multiple times, crystallized with heptane, and it is as white as salt when in powder form. Although I believe that it is rather pure, I still notice that the DMT first crashes out as a orange/yellow liquid form, followed by white crystals. Once the solvent is evaporated, the liquid turns into solid DMT shards with a slightly yellow tint.

Here is an example of the color difference:



Don't get me wrong - I love yellow crystals, just as much if not more than white. However, I'm doing this project to push the limits, to see how far I can go. The crystals are beautiful regardless of the color, but I'd like to see if I can grow a very clear crystal with minimum color.

I believe that at this stage, the yellow/orange crystals are just as pure as the white ones. I thought about the process, and I have a theory about what is happening. The pure "goo" crashes out first because the solution is super saturated/evaporating/cooling down, but it is still above the melting point for DMT. From memory, I think I noticed that when it is cooled quickly, goo is minimized, and the opposite when cooled slowly.

What do you guys think? If this is correct, what steps would you take to minimize the liquid from crashing out? Would desaturating the solution work? Maybe dissolving the DMT into the heptane at a temperature closer to the melting point?



I used to want to achieve all white, and was hell bent on it too, but i wouldnt change a thing right there,, Orangey mounds with whiter Xtals throughout is like hulk hogan "white Brother"
 
blue.magic
#5 Posted : 3/6/2018 1:54:47 PM

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I just wanted to make a post about the exact same problem.

I tried to remove oils by re-x in heptane but this is not very effective. The oily ponds however precipitate quickly and it should be possible to separate them with some loss or simply move them to a smaller area or to a corner.

Although pure DMT has a yellowish crystal form (can be mistaken for impurities), I was able to make white-only crystals when de-fatting with naphtha, heptane or DCM.

I am looking for another route to remove impurities, possibly by a mini-A/B with defat (to save solvent) or FASA using acetone or NPS to wash impurities off the fumarates.

I will also try purification by sublimation, this might be most promising as the impurities will evaporate at mush higher temperature than DMT. Maybe the temperature can be controlled using separate dish with a thermocouple in it.

The main reason for removing oils in my case is to get hard crystals so they can be crushed to powder and vacuum dried (to remove traces of solvent). The powder form will be also easier to weigh and cleaner to vaporize.
blue.magic attached the following image(s):
IMG_20180306_133318.jpg (129kb) downloaded 251 time(s).
 
tydel24
#6 Posted : 3/6/2018 6:36:51 PM

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thats a beautiful sight there Blue,
ive been outta the loop for a bit now,, few yrs since my last xtract,,
your produce sure sparkles! i could never get it shiny like that, i did pull all white pretty much though,, it got asmalltinge after a few days and got darker with oxidization,
i dont think the all white has any of that pizzaz from when i first blasted, ive been chasing the dragon ever since, and ive yet to be able to recreate the events or even come close to how extreme that one went down.. you must know the season well enough with your Vends! maybe thats something i should have taken into accuont more

 
tydel24
#7 Posted : 3/17/2018 7:05:58 AM

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love to read a trip report on that right there! excuse me if this was aforementioned but species was it from?
 
blue.magic
#8 Posted : 3/17/2018 9:55:37 PM

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This is beautiful.

What helps me to get larger and purer crystals generally is to filter the solvent througha bed of Celite (food grade diatomaceous earth will do, but need to be washed with the solvent of choice, say heptane, to remove dust) and then heat the solution to dissolve micro-crystals, the less nuclei the less chance of trapping impurities.

I also wash the crystallizing dish with distilled water and oven-dry before pouring the solution in. With harmalas, I even have to scratch the dish with glass rod to induce crystallization.

It seems to me heptane tends to push DMT out of solution more easily than naphtha, so the slower cooling the better.
 
DrSeltsam
#9 Posted : 3/19/2018 7:55:50 PM

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Recrystallisation has its limits when it comes to purity. Some chemicals can't be separated using recrystallisation or you need weeks to find out the proper solvent mixtures.

I have two ideas:

1.) You could try to use cholacol to bind the impurities once you have the material in solution.

2.) You have to go for a different method of purification. Column chromatography. You can test different solvent mixtures before using a DC plate and then work in batches as the amount you have will overload any normal column. This will probably give you a super clear product but it is quite expensive to do.

You want to practice on something where you don't mind loosing anything. The first few times I did this in a lab were big fuckups.

Perhaps this helps?
 
Silly(c)One
#10 Posted : 4/21/2018 1:26:28 AM

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Back then when I was extracting (2012-2013), I experimented quite a lot with STB & Rx.
I had pure lab grade hexane and heptane, but never managed to get completely white crystals.
The only time I managed snow white crystals was with a full A/B (with lots of defats).
The yield was of course lower than usual but the purity was amazing.
The trip was quite different than my usual spice, softer, less 'tzing', paler colours.
Interesting but eventually (besides the value of learning) not worth the time investments nor the loss of yield compared to STB (+Rx if needed) for me.
 
blue.magic
#11 Posted : 4/21/2018 2:34:25 PM

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Silly(c)One wrote:
Back then when I was extracting (2012-2013), I experimented quite a lot with STB & Rx.
I had pure lab grade hexane and heptane, but never managed to get completely white crystals.
The only time I managed snow white crystals was with a full A/B (with lots of defats).
The yield was of course lower than usual but the purity was amazing.
The trip was quite different than my usual spice, softer, less 'tzing', paler colours.
Interesting but eventually (besides the value of learning) not worth the time investments nor the loss of yield compared to STB (+Rx if needed) for me.


Actually pure DMT has two crystal forms, one is off white to yellow. So color is no longer a sign of purity.

What worked for me every time to remove discoloration, though, was an activated carbon wash (in boiling heptane, then filtered through thin bed of Celite). This is a lossy step and one must be willing to sacrifice some spice and wash everything with warm solvent to minimize losses.
 
 
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