So i just had a batch of RSO syringes fail Phase III (California) compliance testing for residual solvents. (Ethanol and Acetonitrile) it didn’t make sense to me, but maybe i might be overlooking something? Here are the lab results: (GC/FID w/ Headspace Analyzer)
I had to look up what Acetonitrile is, because we don’t use it in our lab. After doing a little research, i discovered that it’s a commonly used solvent in gas chromatography? Just so happens that all of the residual solvents that were detected on that test are used in gas chromatography. Coincidence? Hmm…
Now let’s address the ethanol. I’ve been utilizing the Gemstone decarb SOP with great success up to now. Every batch passed all compliance testing with flying colors this whole year. I’ve been decarbing over a hotplate stirrer for an hour at 130c. Now i was under the impression that my temps won’t exceed 80-90c until all the ethanol has been purged. Is it even possible to have any residual ethanol remaining in a fully decarbed solution? The only thing i could think of is that i did have a fan blowing towards the decarb station to keep the vapors moving as they boil off. Is it possible that the cooling action of the fan blowing on the surface might’ve prevented the ethanol from evaporating? This was a 710 ethanol extraction of 10 lbs of starting material extracted with a CUP15, ending up with about 700mL in a 2L glass beaker.
It’s worth noting that we did do an R&D test (from a different lab), and it came back with ethanol levels ND. This lab was using GC-MS.
Please correct me if I’m wrong, but am i mistaken for thinking that mass spectrometry is better suited for ethanol detection over flame ionization detection?
So here’s the fun part. Here in California, all testing labs automatically report test failures to the BCC so now we have to submit a corrective action plan, and then request permission to remediate this batch to resubmit for testing. Fun times! Have any of my fellow licensed manufacturers in California had to deal with this yet? Not sure we can even go with another lab at this point to retest. The law is setup to prevent us from shopping labs once a sample has been taken, but without any quality assurance standards to hold these labs accountable, what option do we have if the lab is causing us to fail? Any insights or some perspective would be sincerely appreciated. Thanks in advance!