Nope n Ever figured it out. I think it was a lab error because the same terps tested at different lab show no residuals.
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Also chalked our errors up to the lab testing
been seeing more of this happening.
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Hey all, we have suddenly started seeing this happen, never seen this before. 7 years co2 extractions and here is the short story
We extract terps subcritical co2, low temps, freeze immediately at -30 - never have any contact with the ethanol. A recent test shows the Terpenes alone testing at 5000 ppm at the lab -
Started with testing refined oil post vac oven, and it passed, added terps, and failed. so we tested the terps alone and the tests showed ethanol at 5000 ppm and Ethanol ( we don’t have this in our facility) as well. Do any lab techs have insight on this?
Try a different testing lab.
That is strange.
But this kinda sounds like you do have ethanol somewhere in the facility.
Or did you mean it tested 5000 ppm ethanol and “should be a different solvent” (we don’t have this in our facility)?
Have you ever cleaned your equipment with ethanol?
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Something tells me he meant methanol as the 2nd one. I’ve had amounts of methanol show up in extracts despite not having any in the facility.
At 5000 ppm ethanol, I could see residual methanol in the ethanol being above LOD/LOQ. Even USP grade alcohol is allowed to have 0.5 ppm methanol present in it.
Its very likely one of the possible hundreds of terpenes in cannabis has a similar retention time to ethanol on their testing methods.
Could be a mix of poor testing methods or the more likely possibility of their test time is reduced to give more tests per day but in turn the separation of terpenes is reduced and in some cases has some overlapping retention times.
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Sorry, my typo and poor proofreading -
We do not use Isopropyl alcohol not even for cleaning. - we do use ethanol, for Winterization and cleaning regularly since we opened in 2014. For the last number of years we have never failed a test for more than 1000 ppm of ethanol, the usual result is ND (Not Detected)
In this last test BOTH Ethanol and Isopropyl were detected. My question is if anyone has experienced terpenes triggering instruments for Ethanol or other solvents, as what the sk8midget is suggesting - thanks any more info is welcome!
From Sk8midget
It’s very likely one of the possible hundreds of terpenes in cannabis has a similar retention time to ethanol on their testing methods.
Could be a mix of poor testing methods or the more likely possibility of their test time is reduced to give more tests per day but in turn, the separation of terpenes is reduced and in some cases has some overlapping retention times.
We do “rush” our tests as we often need oil so quickly - this is a great start. Please keep em coming our orders are stacking up and were locked down by these test results. Peace.
Thanks we do “rush” our orders frequently. The lab charges a premium to get them back in 24 hrs. Our last attempt was we tested the winterized oil before we reintroduced the terpenes and the oil passed. We mix in the terpenes and then it failed, we test the terpenes alone they fail (all “rushed” tests), so we are sure its happening in the terps but we don’t use ethanol in any step of pulling the terps off with subcritical extraction. the machine is clean, dry, etc. it is so frustrating, and we only have one lab within 4+ hrs. We trust the lab, and have worked with them for 7 years, so trying to find suggestions that they may not have considered. thanks again - Peace.
You rushing the lab test probably isnt the reason they are failing. I’m talking about their actual test method being rushed. Some methods will be 5-10 minutes long having peaks very close together. then some methods are longer than 35 minutes which would space out the peaks more and give better separation.
If you are saying the terpenes fail the RSA can you explain by how much? You should be able to do some simple math and see if adding those “hot” terpenes would cause the rest of your product to fail.
Does you lab have GCMS? Have you replicated the results with another sample?
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There are not any terpenes in cannabis that would have nearly as short of a retention time as ethanol so I’d be concerned if a licensed lab somehow mistook the two. Closest thing could possibly be a couple of the commonly occurring aldehydes but I’d wager it’s literally just carbon dioxide and the lab just goofed.
I think any aromatic compound in general would be unlikely, especially at 5000ppm because that’s way above what it would be for anything comparable that’s going to be there naturally (aldehyde, alkane, acid etc). Especially not in CO2 terpenes which are pretty much devoid of these things. OP, do the results show any CO2 in the finished product or terpenes already?
Maybe acetone or ethyl acetate if those are handled in the same space. I’ll bet a whole pizza on it being one of the above. It also could legitimately be ethanol and you’re not accounting for another variable at play. If OP needs help ruling out one of the aldehydes/super stanky chemicals I can show you some data to compare to. But at a whopping 5000ppm you wouldn’t really see anything up there naturally that didn’t come from the extraction process. The things that could be potentially misconstrued as a solvent usually show up at more like 100-1000ppm.
But I’m just a stoopkid.
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I think he is adding botanicals to his co2 oil and having poor results
I didn’t see this was in reference to your terps. It’s carbon dioxide.
Negative - your referring to aftermarket terpenes, AKA True Terpenes, etc. unless I am misunderstanding you? We do not use aftermarket / botanical terpenes, for numerous reasons, we explored that method of flavoring 5 years ago and opted against it as the supercritical was providing a fairly strong terpene profile for the market at the time. Times change… Our terpenes are batch derived, strain specific, extracted at subcritical specs immediatly prior to super critical extraction of the same batch of decarboxylated material. The Terpenes are kept on ice until rotovape winterization and final vacuum oven ethanol extraction are complete. We only add the terpenes we extract to the oil from the same batch, it produces a great finished product. If you have any other ideas, let me know. peace.
Hey Kid - much appreciated, I am hoping we can isolate the inconsistency at the lab. A newly purchased or calibrated instrument, a fresh employee, a new SOP, or whatever really, we just need to get back to passing consistently. Ill keep the thread informed of what if anything we figure out, we got a handful of tests in today to continue to isolate what is causing this. Peace.
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I’ve had it happen. It confused us too
Were you able to isolate the source or reason? we are just throwing some tests for oil, terpenes, and thinking about freeze drying the terpenes before testing. Any thoughts?