The Art of DMT Crystallization, Part 1: Crystallization Basics and Intro to Crystal Design

[Samvidbuho]

Hello forum friends,

I'm compiling a series of crystallization notes that I've been working on while figuring out the results of the solubility studies I posted a little while back.

What I've discovered is that DMT can exist as at least 3 polymorphs, which was pretty exciting to me. I was hoping to discuss this earlier, but the task of explaining everything has been difficult to say the least. I had to read 17 articles or something like that on polymorphism before I learned how to read the solubility curves well enough to explain this trimorphic system, and the total number of articles I've read on solubility curves in general is somewhere like 35-40+.
I realized that the post I put originally on DMT's solubility was incomplete -- there were a couple of anomalous points that I left out intentially, thinking they were wrong, but they were actually correct and I had just misinterpreted them. So I felt a little remiss about leaving that open too.

I really love this forum, and I used to learn everything on here back in the day, so now I'm happy to give a little something back that I'm, well, pretty proud of in truth. I didn't want anybody to be at a disadvantage if I were to talk about enantiomers and monotropes, transition temperatures and kinetics of phase changes, so what I decided to do is start from the beginning and create a guide to crystallization that I think will prove extremely useful. (I mean, who DOESN'T love the crystallization process, right?)

I did my best to break it up into digestible 1-page chunks of different topics, Part 1 dealing with crystallization basics and building up to how the crystallization process is controlled and Part 2 dealing with the practical aspects of DMT crystallization and how to really control the process and design crystals the way you want.

The topics in this series are the following:

I. Crystallization & Supersolubility
II. The Solubility Curve
III. Nucleation
IV. Crystal Growth
V. The Metastable Zone
VI. The Metastable Zone Width
VII. Mapping the Crystallization Process
VIII. Seeding
IX. Theory of Crystal Control

For fun I included three of the graphs that I think are the most important, yet will be discussed in Part 2. But you can see how the curves of the three pulls I did come together to create this trimorphic system.

Hope you enjoy

 

[Laughter.]

Just curious why 65 and 95 are empty in terms of solubility

 

[delocyd]

How do I get to whole article? I am a technotard.

 

[neurobloom]

Awesome work! Is there such detailed experimentation on 5-meo-dmt crystalization? Funny enough I've had harder time trying to crystalize clean 5-meo-dmt vs dirty 5-meo-dmt.

Even when it crystalizes its always partially oily.

 

[Icon]

Awesome work! Is there such detailed experimentation on 5-meo-dmt crystalization? Funny enough I've had harder time trying to crystalize clean 5-meo-dmt vs dirty 5-meo-dmt.

Even when it crystalizes its always partially oily.

Have you had any luck figuring out your oiling-out issue?

Hi btw, I've read a few of your posts that were really outstanding and helped me understand some things. I'm glad you still come around here too, hopefully I'll have a chance to help you in return.

The crystallization process is something I'm interested in breaking down and learning all about too. I don't have any experience with 5-meo, but in general oiling out seems to be an industry-wide issue. I watched this two-part series by Mettler Toledo where they reviewed a study of the nucleation process for a compound. They use a laser to count particles in a solution and measure the size distribution. They measured an oiling out event, a sharp drop in the # of fine particles as they coalesced into oil droplets. In the end, I think the only adjustment they made was increasing the quantity of seed crystals. The increased surface area available for growth was sufficient for the solution to discharge the solute without oiling out.

I didn't want anybody to be at a disadvantage if I were to talk about enantiomers and monotropes, transition temperatures and kinetics of phase changes, so what I decided to do is start from the beginning and create a guide to crystallization that I think will prove extremely useful.

I don't think I'm quite there yet but we're definitely on the same path. I hope we get to talk.