Forgive my naivety here posting as I’m relatively new to the forum here, but have searched ad nauseum for something relevant posted and could not find anything.
I’m currently a lab tech in an extraction room in a newly(ish) rec legal state. Recently, we bought a large order of distillate. When we received said order of distillate, something like 15 or so liters of said distillate arrived in broken liter jars. You could imagine the mess, little glass shards mixed in with an obnoxious amount of disty, not a fun clean up. The tainted disty was mixed with ethanol and subsequently ran through a large buchner in several batches to remove the glass, now being ran through a rotovap in order to remove the ethanol from the disty.
As the “final product” disty has been removed from the rotovap and let sit for a few days as this is my life for the foreseeable future, I’m noticing the consistency isn’t getting to a point close to what it was prior to mixing with ethanol, and the color has changed to a significantly darker shade. I’m also noticing a slight, slight odor of ethanol still after removal of the disty from the rotovap. Is this normal? Should I be concerned/thinking about running the materials through the machine again?
I’m running a 5L rotovap. Water bath is set at 55C. High 40s low 50s RPM rotor speed. Cooling pump set to -13.5C and generally fluctuates 5 or so degrees under after it hits it’s set point. MPa is at a constant -.09
The first two batches were ran for a hair more than an hour, since then I’ve been going closer to an hour and a half to an hour forty five.
Any insight or advice is greatly appreciated. Thanks in advance
Needs to be re-distilled, you’ll never get it back to the same color with a roto. You’re ethanol % is probably not passing either. EtOH affects distillate color when left in solution for appreciable amounts of time.
So your comment brought up something that I forgot to mention in my post but, being that we are a licensed legal op, everything that ends up being pulled out the rotovap will end up being tested prior to using in product.
We were planning on using this material for gummies, so getting it back to it’s original state isn’t the biggest concern ever, I guess it’s more so like, is what I’m doing going to be more of a headache than useful? If I’m getting a feint smell of ethanol in a jar of 2000g of this post rotovap material, I’m probably gonna have to run it again right?
So whatever is in this massive cauldron of EtOH + disty just sitting waiting to be rotovapped is going to be black as shit by the time I get through all of it?
If color doesnt matter try a drying oven with shallow pyrex dishes. Go as high as vac as you can without making a mess, ramp temperature as needed, keep glass covered from light (probably not going to do much since UV doesn’t penetrate normal glass, whatever, your call) and test again.
If it were me, id re-distill to clean it up and to make 100% sure theres no glass or artifacts from the breakage. @NewLevelProcess is on point with both suggestions
Honestly I don’t even think a buchner is a safe way of remove micro shard of glass, but couldn’t tell you definitively. I’ve had this happen and my choice was always to just re-distill. You’re still likely going to lose 30/40% depending how much you recovered from the breakage. I’d contact the supplier and see what they can do from their end for the shitty packaging.
Re-distill. You may even end up with a higher percentage of THC than the original with the extra distillation. I would contact the company that sent the broken jars and have them re-distill it. I’m guessing you don’t have a distillation machine on-site and that’s why you purchased the liters from this company. The supplier should make it right. Plus, they need to know about the broken jars so they can fix it from happening again.
For future shipping of disty, those 64oz ball jars and jars of similar width fit perfectly in styrofoam shippers for magnum wine bottles. Reusable too.
Wide mouth media bottles also fit in the uline wine bottle shipping boxes with the foam. Literally just shipped 12 liters like this across country and both boxes arrived intact with no damages
I have had The misfortune of having to clean up on multiple occasions broken flasks with multiple kilos of distillate inside which ended up on the floor or on the table… As well as some making it on to the wall and I can tell you I would completely flip out if I ended up with a 30 to 40% loss. I can only assume you had one of your lab guys tell you that’s how much you lost after they cleaned up… Chances are you got screwed.
