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My First Recrystallization

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CloudyDays

CloudyDays

Rising Star
In my introductory post, fink suggested I should recrystallize my spice as it may be impure. As suggested, I purchased some heptane and gave it a try. I followed the procedure on the wiki, except for the carbon step. I measured out a bit over 0.5 g of spice and 30 ml of heptane. The jar with heptane was placed in a bath of near boiling water, then the spice was added. An orange material stuck to the bottom. The heptane seemed to be evaporating quickly, so I added another 7 ml to the jar.

The solution was then transferred to a clean jar, wrapped in a towel and left to cool for 2 hours. It then went to the frig for 4 hours and then the freezer for 48 hours.

Today I took the jar out and was relieved to see white lumps on the bottom. I poured off the heptane and scraped the material onto a plate. There is a small amount orange material in there. I dried the material with a fan for a few hours. Ended up with 0.436 g.

I am really pleased with how it came out and it was fun taking a few baby steps into the world of organic chemistry. Now I just need to try it out!

Questions:
- what is the orange material? Should I save it?
- What should I do with the used heptane? Evaporate it? Save it for next time?
 

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Wonderful job! Those crystals look nicely resolved! I bet that was fun! I'm also a big fan of pictures and detailed posts, so good job there too!

CloudyDays said:
As suggested, I purchased some [REDACTED BY OP] and gave it a try.
Click to expand...

Edit your post and remove the name of the brand, we try not to do that in case a brand gets targeted and banned. At least that's what I have been told. EDIT: OP FIXED

CloudyDays said:
The jar with heptane was placed in a bath of near boiling water, then the spice was added.
Click to expand...

I hope that you turned your stove off before adding the jar of heptane to the water bath, as heptane has a flash point of 20C and is very flammable! If so, add that to your post as well in case someone else is visiting the nexus and decides to copy your recrystallization process.
Harm Reduction = Good.


CloudyDays said:
Questions:
- what is the orange material? Should I save it?
- What should I do with the used heptane? Evaporate it? Save it for next time?
Click to expand...

The orange goo. Goo goo goo. Polymorphs, impurities, oils, alkaloids. I'd like a simple definition myself but... check out this thread and this thread and you should find some answers.

As for the heptane, yes, totally reuse it. You can evap it off if it's a tiny amount or add it back to your heptane container, when I do my multiple 50mL pulls for extraction and then decant it from the frozen dish, I decant it back into the original container. Can be reused and reused.

I have yet to do a re-x, I'm waiting until I have a few extractions worth before I attempt. Awesome job though! Let me know if you notice the difference in your experience as I have only done yellow spice. Some people say the yellow spice has a more comforting nature vibe.
 
I edited the post to remove the brand name. Totally understand the rationale. Thanks for the tips of working with heptane. I didn’t actually use a stove to heat the water for the water bath. My wife had just made tea and I used the leftover water in the tea kettle. But going forward I will make sure to keep solvents away from heat sources.

I think I will save the orange stuff and experiment with it later. Even though it looks ugly, I guess it is good stuff.
 
Beautiful, love that pure white brilliance of clean spice.

I took a picture of some dark orange goo under a microscope. It appears to contain some crystal type structures as well as some plant structures. The perfect round artifacts are air bubbles.
 

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fink said:
Beautiful, love that pure white brilliance of clean spice.

I took a picture of some dark orange goo under a microscope. It appears to contain some crystal type structures as well as some plant structures. The perfect round artifacts are air bubbles.
Click to expand...

Very cool to see a photo of the goo under a microscope! Indeed you can see plant material AND crystals. Right on!
 
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