Ion chromatography is fairly expensive to spend on something unconfirmed, unfortunately.
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Discussed briefly up thread.
Can probably be baked or washed out. Then hopefully analyzed.
Some things won’t fly in a GC.
Some won’t burn in an FID, others can’t be seen with a DAD.
Even if ”it” can or does, that doesn’t mean we are any closer to WTF is this.
Certainly on MY list of todo’s
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Fair point. A non-miscible contaminate would tend to stratify towards the top or bottom in storage containers: the manufacture’s, the fill plant bulk tank, and I suppose, even in the cylinders that are filled.
The degree of miscibility and inclination towards stratification could be determined once the contaminates are identified. Such chemistry is above my pay grade, but could be accomplished once the contaminate(s) is/are identified.
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@TheWillBilly , Since you and I have never been able to discuss your methods, and since there have been no reports of unknown impurities in your products of which I am aware, I can only assume that you have been able to create your polymorphs of THCa crystals by varying the chemo-physical parameters around the crystallization, such as temperature, pressure, nucleation, and solvent of the mother liquors. If this is an accurate assumption, then NO, we do not actually know…
Just because the polymorph can be created in some physical way does NOT exclude the possibility of it forming in some chemical way. After all, MILLIONS of different elements and compounds can crystallize, yet their morphologies are often IDENTICAL. Only about 20 crystal shapes have been classified in just 6 or 7 natural crystal systems, as seen here: What are Crystal Systems and Mineral Habits?
Perhaps we are saying the same thing, and I am just reading your message incorrectly…? If your THCa crystals in the “rectangle” polymorph do not become chalky, the difference in chemistry of crystal growth should be obvious to you, already. The “instability” is literally just that: a molecular instability! 
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@GasGuy-QEG , thank you for your post explaining gas filling, and your other helpful contributions to this thread! Also, just fyi…
I think this DOES make sense to you. After all, your three (2) explanations adequately cover it! 
@_joe , just a bit further on your comment…
While it is usually adequate for a LOT CoA value to be taken from the stream of liquid entering a tank, this value would NOT account for any potentially soluble/mobile contaminant preexisting inside the empty cylinder. Do to the phenomenon of settling/separation in mixtures (as @kromatik1 mentions), the most accurate sample for a cylinder CoA should be taken immediately after filling the cylinder, while everything is still well-stirred and homogeneous. That being said, BOTH CoAs (and even a few others, all equipped & standardized for EVERY potential trace contaminant, such as amines) would be required to locate the source of the contamination.
@dunewalker , I genuinely appreciate your mentioning the soluble ammonium salt foliar fertilizers! Although @cyclopath says, this could be the cause for “some but not all” cases, I believe this could relate back to the cylinder contamination, discussed earlier… since some facilities employ the HORRIBLE practice of using/recovering their solvent directly into & out of the distribution cylinders! 
It is a fundamental principle of good laboratory practice and chemical hygiene: NEVER put UNUSED or RECYCLED chemicals BACK into the STOCK chemical vessel, whether or not any stock chemical remains… especially NOT WITHOUT RELABELING the vessel, accordingly! 
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AHHH…somebody has his thinking cap on…
Everything you say is “right on target”….but you are thinking
Crystallization from nonpolar solvent mode…not solubilization.
For a year or so I have been stressing the exact same thinking mode
In ‘Butane works but no theory”…
When you stress the weak acid nature of the R-COOH of THCA…
You are not stressing the salicylicate nature of the acid as well…
Which complicates things further.
This is NOT a regular carboxylic acid anion.
In aqueous…the pKa of THCA is
3 . And Yes is does dissociate in aqueous. If you buffer it to pH 6.5 it is readily
Ion paired and bound to SAX resins…which is a standard preparation procedure
Published by Agilent. (BTW SAX are quaternary Ammonium…heresy?)
However, the pKa for Salicylic acid in non polar alkane
Is more like 11. so yes, when you are talking about precipitation (crystallization from Butane) your analysis is correct.
When we think about butane extraction to butane precipitation…we have vastly different solution matrices.
If you look in the list of total know extractables from the trichomes you will find
Palmitamide present in almost equimolar concentrations to cannabinoic acids…
And the amides can and do provide ion pairs as you suggest.
If it is not an amide or amine or a Hydrogen ion ….the ion pair has to come from somewhere….in order for BUTANE TO WORK AS A SOLVENT in the first place.
THCA is not crystalline in the trichome…how can it be highly concentrated in the
Trichome…and then Extractable into alkane…only to crystallize spontaneously from butane?
Clearly the problem you delineate is thinking non-polar solvent…chemistry.
And you are on tract…aprotic-nonpolar.
How did the THCA get into that environment in first place?
What does it mean to have CANNABINOIC ACID IN BUTANE?
Below contains a 30 page introduction/guide to how a Ph.D.
Chemist might begin thinking about the subject.
The original thought …of extracting from semi-aqueous (terpene as detergent) soup
In trichomes…where the pH is about 5…then we would think
The RCOOH salicylic acid moiety should be half ionized in the terp-soup trichome storage…and maybe we are extracting BOTH FORMS as a ternary Ionized pair with some bound water. [Trying to think in the simplest terms and explain all observations)
It is possible your RCOOH is actually binding the anion RCOO- (as a substitute for weak base amine non protonated) and carries a water molecule or two in a complex extractable (from terpene detergent soup) by the Butane at -40C.
This falls apart in dilute alkane where the pKa is now 11 forming two RCOOH molecules and robbing a H+ from the water.
{{ [HA]—h—{A-}—H— OH}}. Ternary, non polar h-bonded solubility complex…at -40 (FROM terpene soup).
Technically speaking , a heterologous DIMER MONOHYDRATE.
So precipitates out as homologous-dimer crystals after robbing water of H+ ion.
To me this is most simple explanation of butane solubility.
The second would be an amide playing the role of the amine you suggest but in extraction side, but not necessarily in the precipitation side (crystallization of dimers).
Third may be the Plant pumps Hydrogen ions into the trichome storage area sufficient to Pair each Cannabinoate with and hydrogen ion…and form a butane-extractable R-COOH.
Now in technical terms, it would be the direct extraction of
Homologous-Dimer hydrate. Remember this is aprotic Butane;
But when shifted to protic formic-water-methanol solvent
For RP-HPLC with MS analysis…returns the “happy-form”
That everyone wants to think about: monomer, unionized THCA.
The non polar alkane solution your are thinking about is far more complicated to begin with…and you are thinking about amines from Gas tanks complicating an already complicated solution which for some reasons wants to precipitate THCA
With or without the gas tank contaminates.
A while back I posted a thread: https://future4200.com/t/re-cocrystals-and-salts-cannabinoates-in-never-never-land/174502/10
This provides a modern interpretation of your carboxylate salt chemistry review.
I hope everyone appreciates the deep thought you have put into this subject.
Above I am just “throwing out’ some additional ideas that might stimulate more thought. None of which negate your proposed schema.
Finally it seems we have a discussion of the cannabinoate acidity-ionpair-salt concept. …in PROTIC, in APROTIC and NONPOLAR solvent environments……
With cannabinoates morphing into different forms depending on the environment.
and yes…it has something to do with Pka’s …and “over-thinking”…and sarcasm. ( The latter having nothing to do with your post).
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For what its worth, and without naming names, there is a company that provides one of our client customers with non internally treated cylinders who experienced “Medusa” stones in various severity, doubtful they’re the only ones…
So if its a cross-contamination source from internal treating probably from the transport carrier cleaning SOP?
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Wonderful stuff, the last link at the bottom also shows some reactions that can occur. Thank you for sharing.
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You’re welcome, I got in the rabbit hole reading a sulfate free shampoo bottle, then Google butane with sulfates, then diethanolamine. . Which seems to correlate with alot of information in these two medusa type threads…
It’s used as a foaming agent in cosmetics, and also an emulsifier which are sometimes used for certain types of foam.
It can be solid white crystals, or oily liquid.
Also water soluble
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Just wanted to share, 5 day growth on these. This was a fast crash/Medusa batch, chalk was noticeable within 36 hours of being in a vac oven and a sample left unpurged in a jar.
Let me know if anyone has other questions about the parameters.
They were so pretty at first lol
Not sure if anyone in the pdx area has access to testing for this, but I’d be happy to donate some test samples.
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It’s so frustrating seeing the beautiful stones chalk out
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I only know of one rule about OG Status: Never, ever apply it to yourself.
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This one is interesting, even forms an azeotrope with propane, an everywhere I look into it, says it’s only removed to some degree.
By all means shoot it down
Ethyl fluoride.
.another one that is removed via activated alumina
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Curious if anyone has noticed melting point changes with the Medusa diamonds?
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Yes much higher melting point, or at least its been much more temp needed to make decarbed thc
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Saw similar stuff myself… 250f and its just fine (multiple hours)… used to start decarb at 180f within the first.
This is quite significant I would think. The molecule has been altered from its normal state, as for the melting point to change the molecule must also change.
Edit: Carboxylic acids are quite reactive and could be getting modified during extraction by an impure gas.
2nd Edit: Typically, to increase the melting point, a product with an even higher melting point needs to be mixed in or added to the lower melting point product. At this point, the melting point becomes a value on a number line between the two based on its percentage ratio.
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We used to decarb 180-200 and now always 240+ and much longer. Wonder if the potency changes as there was talking the the willbilly thread that he can control potency via different polymorphs.
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Growing crystals under electrical and/or magnetic fields has been shown to increase the x-ray crystal diffraction quality of many samples. By introducing a filed to align to, the crystal is given structure before it forms and no longer follows the random method of the standard model. Since crystals are aligned by charge in nature, they will align themselves to the induced filed(s) during growth / formation phase which then increases the final crystal quality upon complete growth.
So yeah, you can increase purity with different polymorphs for sure. 
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Monomers, dimers anhydrous
Monomers, dimers monohydrates
Monomers, dimers di-hydrates
Mixed permutations.??
If you melt a crystalline form and it re-anneals as an amorphic- glassine state.
would you not expect the same pure material to have a different melting point?
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