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My First Recrystallization Options
 
CloudyDays
#1 Posted : 2/15/2023 12:40:22 AM
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?
CloudyDays attached the following image(s):
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IMG_7770 copy.jpg (916kb) downloaded 66 time(s).
IMG_7804.jpg (2,557kb) downloaded 66 time(s).
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Toshido
#2 Posted : 2/15/2023 6:06:28 PM
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 wrote:
As suggested, I purchased some [REDACTED BY OP] and gave it a try.


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 wrote:
The jar with heptane was placed in a bath of near boiling water, then the spice was added.


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 wrote:
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?


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.
🌳👨‍🔬🌳 - My A/B Hot Plate TEK - 🌳👨‍🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
✴✴✴ - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
CloudyDays
#3 Posted : 2/15/2023 9:00:54 PM
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.
 
fink
#4 Posted : 2/15/2023 9:23:07 PM
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.
fink attached the following image(s):
20230115_120012.jpg (2,355kb) downloaded 49 time(s).
I don't know much, but I do know this. With a golden heart comes a rebel fist.
 
Toshido
#5 Posted : 2/15/2023 9:57:11 PM
fink wrote:
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.


Very cool to see a photo of the goo under a microscope! Indeed you can see plant material AND crystals. Right on!
🌳👨‍🔬🌳 - My A/B Hot Plate TEK - 🌳👨‍🔬🌳
🍜🍜🍜 - Don't Heat Your Naphtha, Heat Your Soup! - 🍜🍜🍜
✴✴✴ - White Spice vs Yellow Spice - 🌟🌟🌟
"You are an explorer, and you represent our species, and the greatest good you can do is to bring back a new idea, because our world is endangered by the absence of good ideas. Our world is in crisis because of the absence of consciousness." - Terence McKenna
🙌 "Dang, that's really impressive for a first extraction. Those xtals are nicely resolved." - Benzyme 🙌

 
Pandora
Welcoming committeeSenior Member
#6 Posted : 2/25/2023 7:41:53 PM
CloudyDays,

Great job. And those are some gorgeous pictures of some fantastic crystals. Thank you so much for sharing.

-Pandora
"But even if nothing lasts and everything is lost, there is still the intrinsic value of the moment. The present moment, ultimately, is more than enough, a gift of grace and unfathomable value, which our friend and lover death paints in stark relief."
-Rick Doblin, Ph.D. MAPS President, MAPS Bulletin Vol. XX, No. 1, pg. 2


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