3% hydrogen peroxide solution mixed with stable butane did nothing but cause some offgas from the heat provided by the water/H202.
My working tank was initially definitely more volatile than the stock tank for the first 45 minutes and then for the next 1-2 hours, the working tank was more stable than the stock tank.
I have seen chalking with both 70/30 butane/propane and 60/20/20 butane/propane/iso-butane. I will say the issue seemed more prevalent during the time we used 60/20/20 but I don’t think iso-butane specifically is the source. Observationally, based on the stock and working tanks, it appears to be a low-boiling impurity because I don’t know what would react with butane or propane to produce an offgassing reaction without catalysts or very high temperatures. Of course I could be wrong.
I also agree that warmer crystallization Temperature and staying on top of molecular sieve use helps reduce the issue but we have a lot more work to do to get all the answers.
We got solvent analysis done on our 13x molecular sieve and did notice a couple of out of the ordinary solvents (81 ppm acetone and 919 ppm isopropyl alcohol). We did however wash the sieve with denatured ethanol and didn’t regenerate it at high enough temperatures, so there was plenty of Ethanol (52,325 ppm) in there, which pretty much invalidates the results due to cross-contamination of solvents. More COA’s coming soon from the 13x molecular sieve.
I have to look at my notes, but I took the average density of stock and working tanks (my tools were not perfect for measurement so averages will suffice for now). Working tank was a tad bit higher which is to be expected due to increased butane and terpene content vs the stock tank.
@hambread : Your preliminary work with the 13X suggest someone is going down the right path. Dm me if you need any thought/discussion about appropriate controls.
I’ve been trying to get local labs like BelCosta and Cannalysis to add to their solvent testing capabilities. BelCosta was receptive to this idea and we specifically discussed both propylene and neo-pentane - however no action yet has been taken on their part and it has been months of discussion.
If any labs are willing to put resources towards this NOW, please message me.
Let me guess, new tank of gas. Running product that you’re familiar with and never had issues. Then had a sudden violent reaction like this, no gradual buildup of symptoms. Went from normal to this in one run after a fresh distillation out of a new tank.
There seem to be some problematic aspects of analysis of
low MW alkanes …https://theanalyticalscientist.com/techniques-tools/its-all-about-the-residue
In addition to propylene and neo- pentane, there is a whole world of low level diamandoid contamination…(mystery oils) of LPG, butane etc… that no one talks about.
Moreover, I think you may need a special quadrupole scan selection SIM focused on low molecular weight.
Not every lab or any lab is going to do this for you.
I feel like we are beating around the solvent issue bush right now, because certain labs will get shut down once they realize this is a solvent issue. It is a more prevalent issue then is being lead on. I feel like They are well aware of the issue and don’t want any blow back. So in my mind try and point out anything it could be besides the solvent. That’s how I feel at this point. Beyond frustrated, we’ve known it was the solvent since the first weekend it started happening. I don’t know what exactly, although I can say the amount of odor and mystery oil from distill runs is 100x worse then I ever remember it. Smells like hydraulic fluid. 13x and cleaning after every distill run seems to really help alleviate the problem. Not 100% fix but alleviate. Thank you Dred for the original recommendation.
Isopropyl alcohol and acetone never show up in our butane/propane extracted live resin (nor did they show up in the unpurged extract). Typical denature ethanol cross-contamination in our butane/propane extracts would only show ethanol and heptane in amounts that make sense based on the source solvent.
We have had chalky THCa crystals test at 99.7-99.8% THCa and show over 1000 ppm butane (rather than the typical non-detection). I’ve seen residual solvent and HTE seep out of solid THCa crystals after sitting on the shelf for a week, post-purge.