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How can I avoid amorphous precipitation on re-ex with nps?

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swim.nobody

Rising Star
How can I avoid amorphous precipitation instead of crystallising while freezing? I can't find the proper saturation before freezing while re-exing with nps. I evaped until milky white when blowing air but instead of crystals solid dmt is breaking out of solution. The solution is full of dmt but it's not crystallising. Can it be too saturated?
 
Tell us what you did in maximum possible detail and it might be possible to troubleshoot more specifically.

Better crystals are formed with slow cooling and lower initial concentration of DMT - don't heat the NPS (naphtha? Heptane?) too much, best not to exceed the melting point of your DMT. Insulate your re-x container before cooling, and let it chill in a fridge before transferring it to a freezer.
 
I scrapped all crystals after first freezing and full solvent evap. Added as little nps as possible to dissolve all crystals in hot bath. I let it cool and observe lot of dmt breaking out of solution as small points. The solutions was intense milky white without any blowing Put in the freezer but all dmt was floating as in room temp. Took the dishes out added more nps to the point of clear solvent and evaped to the point of milky /cloudy white solvent . Re put in the freezer now it precipitated as dense powder but no crystals.

Even though I have airtight dishes I will not use the freezer as I have small kids. So nope. For the freezer I have a separated one that goes to - 30 degrees
 
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To avoid amorphous precipitation and get proper crystals while freezing with NPS, make sure the solution isn't too saturated. Before freezing, evaporate the solution slowly until it becomes slightly cloudy, not milky white. If the solution is too saturated, DMT won't crystallize properly and will form solid chunks instead. So, find the right balance by evaporating gently until you see the first signs of cloudiness, then freeze.
 
I have observed that slow evap works the best for growing big chunks.
The slower it evaps and the more time the solution has to grow, the better the crystals will evolve.
Never tried to put the solution in the freezer in the middle of the process but I think that would speed the crystalization too much.

I take a small 50ml container, put the dmt in it, add a few ml warm solvent.
Then mix the solution and make sure that all the dmt dissolved.
If it did not then I add more solvent.
Take a tin foil, make holes in it then place it over the 50ml container.
Now do not touch the container for 7 days.
During the process the solvent will evap very slowly and on the edges of the container some crystals should form.
The more evaps the more xtals will continue to grow from the edges to the bottom.

If you are curious about the outcome: just some xtals
 
billypeoples said:
To avoid amorphous precipitation and get proper crystals while freezing with NPS, make sure the solution isn't too saturated. Before freezing, evaporate the solution slowly until it becomes slightly cloudy, not milky white. If the solution is too saturated, DMT won't crystallize properly and will form solid chunks instead. So, find the right balance by evaporating gently until you see the first signs of cloudiness, then freeze.
Click to expand...
What the heck is with that link, though? :confused:
 
swim.nobody said:
How can I avoid amorphous precipitation instead of crystallising while freezing? I can't find the proper saturation before freezing while re-exing with nps. I evaped until milky white when blowing air but instead of crystals solid dmt is breaking out of solution. The solution is full of dmt but it's not crystallising. Can it be too saturated?
Click to expand...


Like everyone else is saying try slightly heating the solvent as to increase its solubility and the amount of DMT it can hold then allow it to cool slowly. Allowing to cool slowly will allow for bigger crystal development. Getting your ratio of saturation to the depth and surface area of your container will also be helpful in this. You definitely don't want to evaporate too much from your dish as this will make flatter crystal development but you want to make sure you still have a saturated solution to allow for a good recrystallization to occur so you don't want a wide dish if you are going for more of a snowball rocky crystal form.

I allow my re-x to sit out until it cools to room temperature then place in the fridge for a couple hours and then the freezer and get nice crystal development that way. Also want to make sure you are leaving enough of your solvent in for crystal development to occur which I've found smaller dishes to be very beneficial for recrystalization because you do want the right amount of saturation but don't want to have too little depth to the NPS in your dish or the crystals won't form right.

This link to trillium Tek was also very helpful for info on understanding growing crystals a bit more.

Trillium Tek growing large rock like crystals


Here is another helpful video on this subject that also kind of helped solidify what is going on here in my head.



Recrystallization is a very similar process to making rock candy




Hope these links can be helpful OP!
 
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