just some xtals

[AlchemicalGnostic]

on my last extraction, I set the last pull aside to evaporate instead of freeze precip. I put some fb from my last extraction to create a seed and got my very first crystal! not that impressive compared to these others on this thread but I'm proud of them

 

[Jees]

^^^ very familiar looking crystal shape.
Very impressive!

These are smaller and precipitated out of a backwash using ammonia to base:

 

[AlchemicalGnostic]

Oh wow those are pretty little guys!

 

[Orion]

Just some notes...

I believe the clouding of over-saturated dmt pulls impurities downward as it precipitates. I allowed this to happen first at temperatures higher than room temp (like a slowly cooling double boiler) then separating the hexane away from it for room temp precip. When I transferred this hexane it was clean but cloudy and produced some lovely crystals.

Over-saturation is not good though. The problem with concentrating a clean solution is that it becomes a dirtier solution overall and can precipitate a yield that looks disappointingly similar to the last. It can precipitate too rapidly during cooling even when left in the double boiler of hot water. This causes the precipitation of oil which I believe is just liquid DMT, caused by molecules not forming large enough crystals as they precipitate. The spice must flow... except when you want nice xtals :d

Results were varied using a fan to concentrate hot pulls from the crud, redissolving whatever crashes out under the airflow again using heat and cooling slowly to room temp. It did not do much to clean up anything less than almost white spice. It can be hard to tell when to transfer the naphtha again after oils/ crud precipitate but I think best results were just as it reached room temp, perhaps a degree or two above. Doing this on almost clean spice yielded nice crystals.

 

[DoingKermit]

Beautiful crystals, Orion! That mass in the bottom left corner of the second pic looks impressive!

Interesting point on over-saturation. I've also noticed if I work with warm/hot pulls, I always leave the solvent to cool to room temp and then decant leaving the crashed impurities behind. I used to stick in the fridge for 10/20 mins to aid in the process, but this easily caused loss in yield due to the amount of DMT that would start to crash out with it. These days I don't tend to do warm pulls or fan blow (much) to saturate the solution. Seems to produce cleaner results overall.

I might have to start playing around with crystal growing through slow cooling again, as it's been ages since since I've used the technique. Is that how you grew those big guys? Or was it slow evap?

 

[JustAnotherHuman]

Great crystals Orion!

 

[Orion]

Thanks JustAnotherHuman!

Kermit, these were from slow cooling to room temp after being saturated at a higher temperature. It began to precipitate while still warm but it cleared as it did. I decanted the solvent to another glass, took it to the coldest room and found those crystals in the morning.

 

[JustAnotherHuman]

Must be so nice waking up to crystals in the morning.

 

[Phlux-]

eish photobucket just lost the plot. most of my images on the forum wont display.

 

[Mindlusion]

eish photobucket just lost the plot. most of my images on the forum wont display.

I was hoping you'd find it soon enough When the tradegy struck, opening the front page of this thread just, was not as magical anymore

 

[pitubo]

eish photobucket just lost the plot. most of my images on the forum wont display.

The Traveler changed the forum software. Externally hosted images are now cached by the forum software, so that a local copy is viewed. Unfortunately, images that were posted before the change are not cached.

 

[espurrr]

something from the outer world (not nexus)

 

[third-eye-open]

These are cubes I grew over 2 years ago. I'm currently experimenting with using them to seed larger ones. Ill up date soon.

 

[Orion]

Another musing on re-x...

Yellow naphtha is guaranteed to give yellow DMT if it evaporates. If you you take that jar full of DMT and cover it in a minimal amount of naphtha and add heat it will dissolve. And yet the naphtha is often noticeably clearer when it dissolves without agitation. It takes longer but the impurities are deposited at the bottom where the warm runny DMT was. They don't go easily into solution on their own as they did during the extraction. Some always will mix back into the solvent, and I think this is because of convection currents caused by heat.

I think the majority of the impurities in mimosa extractions are actually solids. I don't recall a single time where I was not able to separate oils (or 'plant fats' as some might say) into just DMT and solid impurities. No matter how many times I am left with an oil, I can always clean it up into DMT and solid impurities, eliminating 'oils' without discarding them.

When DMT crashes out rapidly from solution (as I mentioned in a previous post here) it seems to push a good amount of the oily/yellow stuff down with it. If the impurities are just microscopic solids this makes sense, as they are being trapped by microscopic DMT crystals or globules forming, and gravity simply pulls them down, leaving you with a cleaner solvent which is still saturated with DMT (at the current temperature).

 

[KloudQ7]

 

[Mindlusion]

EDIT:

DMT freebase (synthetic)

hehe

 

[benzyme]

yea, these are some amazing pix in this thread. very awesome stuff

 

[Samvidbuho]

A couple of weeks back I finally took a day to clean out all the glassware from past reactions, which I just let pile up and was beginning to be too much. A lot was unrecovered freebase from post-FASA conversions, and the rest was fumarate salts waiting to be changed. Source material was M. hostilis.

The first picture is the starting materials: The red oil is what was left after acetone (+ little hexane) was used to pull the freebase-carbonate resin, and the other dishes are holding freebase from recently converted salts. These were pulled in turn, and everything combined after filtering with 0.20 um PTFE syringe filter.
(In retrospect, rather than use that oil directly, I'd have recrystallized, or at least mixed it with everything else for longer than I did).

The second pic is the result. Not very pretty, so this was redissolved in 80/20 hexane/heptane, refiltered, and put inside a glass test tube to recrystallize.

The re-x took 9 days for the solvent to evaporate. I wouldn't do it in a test tube again though for the reason that the bottom of the glass is too curved -- impurities which remained as oils during the process gradually slid down the tube, onto the bottom, and were left to interact with the bottom crystal. But I was happy with the side crystal that formed.

The bottom crystal was easy to remove,, was dense, interesting color, but again not really the most pleasing to look at.

So most recently this amber crystal was dissolved in heptane, filtered again, solution heated up quite hot, and upon transfer to a shot glass a tremendous amount of crashing was seen, probably due to the heat loss of the heptane upon contact with the different surface. The crystals were insulated with more heptane, which is where everything is at now. A pretty nice separation occurred, though.. some pretty delicious sunny side up eggs coming through !

 

[Samvidbuho]

Separated the crystals from the last pic, the one with the white crystals has been suspended for 60 hrs without moving from suspension, but the other one has shaped up pretty well..

 

[Samvidbuho]

I'll add another, from a separate batch. Single re-x in hexane, doing FASA method, fairly sure the hexane was used to pull directly from the freebase|carbonate - water solution and transfered directly to crystallizing dish.