Butane Contaminant Demystified

Yea that’s kinda what I’ve been thinking. I’ve had runs back in the day when sieves didn’t get changed that looked like fast crash but would go away right after changing the sieve.

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It’s amazing to me how much collaborative learning there is going on. It feels like the lights just came on and we’re all seeing things that were there, but in the dark. I’m so impressed by the work that going on here. I wish I could just bring in a big tray of snacks. Great job, friends.

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One of the clues was that (essentially) this method does in fact seem to remediate the gas…

Is that the 20yr old GCMS you got up and running? Might have to follow in your footsteps.

The 50 year old HP 5840 that just landed in my lap might be more work than it’s worth (manual seem “rare” at best), but getting a mass spec up would be really useful.

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Nearly EVERYTHING in the abstract here has a corollary in the medusa issue…

crystallized in methanol and water in the presence of simulated structurally similar impurities (Lewis Adduct: THCa-amine is a “structurally similar impurity”)

resulted in impurity entrapment via the formation of solid solutions (THCa alternating with THCa-amine adduct)

Impurities were retained in the solids to a higher degree in the early part of the crystallization and decreased rapidly toward the end (“Catalytic” crystallization mechanism)

impurity entrapment impacted the physical properties of salicylic acid, including its solubility and melting properties (Medusa-petrified THCa crystals are harder to dissolve & melt than typical THCa crystals)

An intra-particle thermodynamic driving force was thus found to exist during the crystallization, which caused selective dissolution of the dirtier cores of the crystal and recrystallization on the cleaner edges (Using higher temperatures can AVOID medusa/fast-crash, even in contaminated solvent)

concomitant but opposing mass transfer processes during the crystallization were responsible for the formation of hollow crystals (“Chalky” THCa crystals are POROUS)

Thanks for the paper, @moronnabis!
I also like your “amine as crystallization enhancer” idea! It might be easier for folks to comprehend than my calling it a “catalytic” process… Yours is a more macroscopic & temporal view where my version is a more microscopic & instantaneous snapshot. To wit, I consider the Lewis adduct to be an intermediate of an unknown but obviously brief lifespan, so this is essentially the same concept, but explained a little differently. Awesome! :wink:

So yeah, @Dukejohnson … This is another way to see it!

Full paper:
wang2021.pdf (10.9 MB)

Diagram of theory from paper:

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Thank you @Photon_noir, this alternative view helps my brain grok the chemistry much better, does the dissolution of the impurities accelerate when a hysteresis of heat is cycled ? The variable always being temperature due to evaporative cooling and atmospheric pressure changes

I bring this up because @Waxplug1 has been expressing his lack of spotting bad gas in other threads and I want to imagine this could be from cycling temps and pressures at a more consistent or slower rate ?

Just a thought

Thx for the gnarly article man :+1:

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It’s not happening in the pot or pour outs either. I wish it did, it would greatly speed up my process

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If by “running” you mean “it makes chromatograms” then yes! If you mean I’ve gotten around to actually doing any quantification with it then no. Unfortunately it got back burnered right after I bought two more lol

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I’ll trade you some gas lol
If I soak, then pour it saturated in the honeypot, prior to flushing with additional solvent I get pretty large crystals floating around, I gotta stop recovery and melt them in when it’s full of solvent less saturated.

It’s usually foggy at the beginning and will immediately go cloudy with recovery set below 75f
At 90f it doesn’t seem to happen as much.

It can literally cold crash using recovery alone if I run and don’t let it occasionally build pressure and warm up, the sight glass fogs over and it crashes into a foggy solution.

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I’m very grateful I haven’t had the fast crash in the collection vessel, but I wonder what differs between us. I’ve seen it in 20 minutes outside of the collection vessel

What temp do harvest at? We’ve been playing with warmer temps on the collection vessel prior to recovery. Also not my choice, but our results lately haven’t been bad (although we also switched suppliers, so it’s not a scientifically controlled observation)

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My current tank seems to be free of the issue.
The last tank which I still have 30lbs of is extra spicy
Thats the only one that has done it in the collection.

I think the main thing for it in collection is how fast you can recover,
/ how hot. if your recovery maintains a vacuum and your vapor path is large it can cool the solution to crashing temps at 85f but at 90f I don’t see it happen.

I have sight glasses on the bottom of my columns, with that tank if I did any soak I could watch it cloud up with thc-a untill I did the 2nd soak which wouldn’t be as saturated with thc-a and wouldn’t be cloudy.

It’s like this fine line of temperature and saturation levels where everything gets spicy.

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Have you considered intentionally contaminating your product with ethanolamine after the pour? I’d be really curious to see if you can make “spicy” gas in your miners with the intention of fast crashing.

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Spicy gas and extra crispy diamonds. why does this make me think of 11 herbs and fried chicken ?

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Kentucky going legal?

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After attending the Medusa roundtable in Eugene, I contacted Isaac Delgado of Vici Metronics for a commitment of support. Vici makes gas scrubbing cartridges and is who I worked with when I was searching for a solution to Mystery Oil.

Isaac offered to supply standard 1200 ft3 cartridges for experiments to remove sulfur and for removing methanol/diethanolamine.

Is anyone interested in conducting the experiments, where you analyze the gas before and after trials and Vici analyzes the spent cart for improvements?

If necessary, I can turn you on to a lab capable of running the LPG gas analysis.

You would also need to run the gas and determine if it solves the medusa problem.

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Is there anyone building a water wash test sled?

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Thank you sir!!

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I am building my water skid today, as a matter of fact. A much better version than my doodles from this weekend.

I would love to try these out, as well.

Not every method will work for every processor. Some may be able to water wash, or vapor wash. Some may have to rely on media.

And I do have some spicy gas in a holding tank. It may have some propane in there but that’s easy to deal with. But, for the experiment, I can make it happen

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My prototypes almost always turn out purdier than my doodles too.

Do I infer you have the design sorted and all the pieces?

If you will email me at graywolf@graywolfslair.com I can get you hooked up for the test carts.

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I will reach out to you today and show you pictures and details of the setup

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sorry to have missed the roundtable, both @thesk8nmidget and myself were out a OCF that weekend.

I’m sure the Chinese rising film sitting in the corner of our C1D1 space would make a great water washing apparatus…but I can’t quite convince myself that it’s well enough built (hey bossman, wanna fill it with water and see if it holds at 300PSI?!?")

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