history tells us to expect THREE Gorgons…
@CallipygianDabs
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Sounds like the new supply from gas logix
I’m thinking this issue might’ve just reared it’s head at my work. I’m wondering if one of the symptoms is higher than normal pressure in recovery but relatively expected pressures in the chilled solvent tank. In other words, the first abnormality I perceived is that solvent tank pressures are generally as expected for the temps, but the pressure during recovery is noticeably but not exceedingly high compared to what would be expected…10 psi higher or so.
The back story…
Recently switched to a new cylinder of Butane. We use it to rich up the butane on our blend depending on products being made…It is not consumed exceedingly fast compared to our other solvents so it could be from a couple months ago…Initially started to notice higher pressure in recovery but recovery/flow itself didn’t seem slowed. If anything, recovery seems fast. I’ve taken apart/cleaned the back end looking for a slowing and found none. Since then, I’ve done two more butane rich runs this week. The first, a shatter run got very oddly reactive in the ovens. Yesterday, I did a diamond run. I dropped the cup cold and wet. When I vented the cup, there was extreme off gassing despite an ice cold cup. After venting to a point, I dropped the cup. As it separated from the column, the cup looked fine. But, a few seconds latter as I lowed the cup, it made a reactive spurt. It was a sort of delayed reaction and quite unnusual from my experience. Looking into my solvent tank, the gas is highly reactive and making a rolling boil at the slightest release of pressure despite being chilled.
Anyway, I don’t have a theory to offer, but that’s what I’ve experienced.
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So you can keep them from chalking with some tricks I think are already a part of your process, but if you just grow the strange facets at a low temp and purge by seperation then they chalk 100% of what I’ve seen. Still think it could be a few things but akin to aerogel as @Photon_noir has mentioned if properly purged you can prevent the contaminant from destroying the structure as it is removed.
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yes. still. unfortunately.
as far as water washing the solvent…all I got is
Is that a solution?
no, they’re immiscible
it’s probably something we’ll try, just for the sake of “ok, can we see anything in the WATER?”. I’ve also got to see what I can get out of our “spent” 13x beads and down the tube to the eternal flame.
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Root Cause Analysis: “Medusa Stones” and “Fast-Crash” in n-butane extraction solutions of THCa from Cannabis, as of May 3rd, 2022
MEDUSA STONES…
Unknowns In Isolate Conversions - Hash and Stuff / Pre/Post-Processing - Future4200
The forum comment above contains a nice illustration relevant to the principles of reaction between ammonia (NH3) or amines and THC-acid (THC-COOH). Although an organic carboxylic acid like THCa is a proton donor (a Brønsted–Lowry acid), it is also a Lewis acid (electron acceptor / electrophile). As you may know, THCa is a very weak B-L acid, because it does NOT donate its proton to water (aka “disassociate” or “ionize upon polar solvation”) in any significant concentration. This makes its Lewis acid character more obvious. That is to say, the ammonia, being a Lewis base, can simply attach to the THCa, forming a ‘Lewis adduct’, like so… THC-COOH4N
This new ‘quaternary ammonium’ compound could be called a ‘zwitterion’ (although this term is normally for a molecule wherein the + and – charges are separated by 1 or more atoms) or a ‘Lewis acid-base complex’ (although usually that term refers to a ‘ligand’ and a metal ion).
I have been discussing ammonia and amines as potential causes for “medusa stones” for quite a while, now, albeit not necessarily on the forum. It is my suspicion that the culprit (i.e., Medusa, the last of the Gorgons) is most likely a highly labile organic amine–probably secondary or even ternary amine–attaching to the THCa to form the “amine THC carboxylate” salt, molecules nucleating and organizing into a crystal lattice structure commensurate with that of the newly formed salt (evident by the macro-crystalline growth & shape of THCa medusa stones being so different from those of pure THCa crystals), then detaching as the energy of the crystallized molecules drops below the energy of solvation for this amine. Essentially, the amine is acting like a sort of crystallization catalyst, thereby remaining in the butane solvent throughout multiple batches of biomass being extracted. This ‘regenerating’ behavior could also explain how the concentration of the amine in the butane is apparently low enough to have escaped discovery by analysis for all this time!
FAST-CRASH…
I believe, although the fast-crash problem may sometimes co-occur with the medusa stone problem, that the two could have separate causes… or at least that these two different phenomena may vary according to the concentration of the offending impurity.
In other words, Fast-Crash could be caused by a different (more rapidly labile and/or precipitous) THCa salt-forming amine… or the fast-crash butane may simply have higher concentration of the salty amine than the medusoid butane. I also believe this problem is further exacerbated by increased concentrations of neopentane in the butane solvent.
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Glad to know I’m not completely insane, thank you! I believe we’re seeing the NH3 and THCA interacting in such fashion that could confirm your theory.
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It is interesting to be involved in these discussions as many of those involved come from different backgrounds and have different perspectives. I want to get to the bottom of this matter too, but feel the group might benefit from another perspective.
I’m an ops director of a gas fill plant that deals with research grade 99.999+% pure rare gases (neon, krypton, xenon), stable isotopes and even UHP helium.
As I look at my Praxair gas catalogue, I see they offer 10 different grades of compressed helium gas. It’s a dirty little industry secret that all 10 of these grades come off of a helium transport holding liquefied helium with a purity of 99.9999+%. The difference between the grades is not in the gas, but in degree of TLC used to prepare / fill the cylinders AND the testing that is required to categorize the gas into one grade or another. If the cylinders are properly baked out to remove all moisture; flushed and vacuumed with UHP helium, vacuumed once more then filled, the liquid helium will retain it’s purity into vapor phase contents of the compressed gas cylinder. So, long as proper filling protocols are followed, the gas being sold as UHP 99.999% purity is the same as the gas being sold as Chromatography Grade at 99.9999+%. I reference this story because there may be some parallels to this situation.
Most hydrocarbon fill plants, receive bulk loads of Instrument Grade hydrocarbons. For normal butane, those loads are typically about 8,000 gallons / 38,000 pounds. That load of gas is sufficient to fill over 300 cylinders with n-butane. More than a full truckload of 225 cylinders.
On this and other threads about medusa and fast crash, posters have written that they receive several cylinders from a supplier. The first one is bad gas, the second one bad and third are good (or some such variation), illustrating that some cylinders are good and some bad.
So, here’s the question: If both good and bad cylinders came from the same fill plant in the same timeframe - - - how could the gas be different ? It’s all coming out of the same spigot. Is the group suspecting that if a customer received good and bad cylinders from the same fill plant, that they must:
- be from different bulk deliveries from the fill plant, and
- that the manufacturing plant changed it’s manufacturing process from one bulk delivery to the next, and
- that if future gas delivered from the same fill plant were determined to be “good”, that they were filled from a subsequent delivery of hydrocarbons where the manufacturer reverted to the old process?
It’s industry standard to put lot numbers on filled cylinders so the fill plant can track backwards to the product in bulk tank(s) when the cylinder was filled. Has anyone ever received a “good” and a “bad” cylinder in one delivery from the same supplier? If so, can the lot numbers be checked?
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Thanks for this info, for the conversations we’ve had in messages, and your engagement with this community. It’s great to have true professionals from all realms.
As an update to my situation, we’ve full cleaned the system and refilled with fresh/distilled gas. For my piece, I can’t tell you if one tank of gas was “good” and one was “bad.” I just know the problem showed up right after a specific tank got put into use.
I am now looking to buy stainless solvent tanks with cleanouts to distill into so we can transfill from those into our jacketed tank PRN without having to stop production for distillation. For our workflow, that seems like a good way to ensure fidelity of gas and not loose time. It seems that the ability to clean these tanks is as important as clean gas.
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Yes I have… the issues goes back to still never receiving any of the COA’s I asked for though. So I have since switched to a different supplier that can provide me coa’s without pulling teeth.
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xenon
Ever huffed that shit? Apparently its an NMDA antagonist…
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i have received cans with varying degrees of this reaction, all react, but with differing intensity. which makes me think the catalyst causing the reaction is not completely homogenous throughout the lot. thoughts?
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I worked with a dude named Hamilton Morris who travels the globe getting high and posting videos under HAMILTON’S PHARMACOPIA. I’m talking about unique highs, licking toads in Africa, inhaling xenon, etc.
I haven’t huffed xenon, but it’s supposed to give a trip. That was back when xenon was selling at $20-30 a liter. 30+% of rare gases come out of Ukraine and the horrible war over there threw the rare gas market out of control. Xenon is now over $120 a liter, krypton is at $13 and neon is at or around $4 a liter. Neon’s primary use is in excimer lasers used to etch semiconductor chips. If you think today’s shortage is hard to handle, wait until neon goes so scarce it closes some semiconductor fabs. It’s going to be awful.
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Is Hamilton Morris as big of a douchebag IRL as he appears to be on TV?
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That doesn’t make sense to me, unless the cylinders themselves were of different chemical profiles. That could come from:
- Residue of hydrocarbon or other gunk that was not removed prior to filling.
- Residue from a cleaning solution that was employed in the cylinder cleaning process used by the fill-plant
- Sorry - there is no #3.
Were the cylinders from the same lot / did they have lot numbers on them?
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We only spoke, didn’t meet him, but he seemed to be OK. Maybe toad licking took a toll on the guy.
I make it a point to make time to go to happy hour & occasionally break free for a round of golf. I can’t imagine taking 2+ weeks off to raft around jungle rivers looking for Peruvian Tree Frogs to lick.
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Hey @thesk8nmidget, tour COA brings up an interesting point. The COA you received is most likely not a COA (Certificate of Analysis), rather it is a COC (Certificate of Conformance) to specifications for the product you are purchasing. Big difference.
A COA is an analysis of the gas IN THE FILLED cylinder you receive. A COC merely states that this is the gas that went into the cylinder you received.
We have received and provided analyses of cylinders AFTER they have been filled. We are though limited in the scope of these analyses. We can only see hydrocarbon species, but that allows us to rule out the presence of ethylene, propylene, benzene, toluene and other such molecules. We do not test for ammonia or amines, as different equipment is necessary and, frankly, there is still much debate on what gremlins are causing these issues. Once we know that, we can explore the source of those demons and most likely develop testing and methods of remediation.
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I’d be curious to see your reaction to my lab’s medusa crashing and how that compares to other peoples. Would you be cool with me sending you some vids/pics and getting some insight if you think it’s unique in any way?
@Dukejohnson and @cyclopath
Would be interested on both of your opinions as well.
It appears to me that our fast crash is much faster than most people’s reactions are occurring, (to my naked eye anyway). Just curious if this is how everyone is experiencing it or if there’s variables in effect for everyone and I’m curious as to why that may be.
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Well a dude in Eugene has an in-line hplc and grabs gas a few times during the fill.
I would assume this is a COA since it came from the same lot and was taken in the middle of the fill
Am I incorrect?
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I’ve seen it crash super fast and slower than super-fast. I believe it may have to do with how clean it is, we ran some fresh frozen bubble that had been squished into rosin but there was a lot left, but it was already clean and then ran the solution through the crc…it crashed out so much quicker than normal, but there wasn’t much terpenes in there
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