I’ve been seeing some mystery delta 10 popping up and for the life of me I can’t figure out how I’m getting it. Looking for some crowd sourced help on this one.
We extract standard THC dry trim material at -20c with 100% butane, no crc or powders.
I decarb the crude between 240-270F
Decarbed crude is then placed into 200 proof ethanol at a 9:1 ratio
Frozen at -20c for 48 hours
Filtered through 5 micron filter papers and roto’d at 65C
Decarbed/winterized oil is placed into a Lab Society 20L short path
I generally go 65c (boiling flask with probe inside) for light volatiles, around 1200 microns depth here
125c for volatiles generally around 5-600 micron depth here
155c for heavy volatiles generally around 2-400 microns here
Ramp to 175c mains, once into main body generally do a final ramp to 181-189c depending on batch and generally between 60-120 microns depth at this point
An 8 L run will produce around 6 kilos of first pass distillate with the entire run taking 8-9 hours.
We are seeing between .6 and 5% delta 10
We saw .6 % delta 10 at 189c boiling flask temp during mains and 5% when doing a run at 182c in boiling flask, with only about an hour longer residence time. TAC coming in around 85%. I’m stumped at this point. Anyone got any spoons?!
Id recommend testing before and after every operation to determine at what point it’s cropping up - that may give insight into what’s causing it. Otherwise, it’s very easy to blame trace amounts of sulfur and heat.
Excellent idea, we’ve tested the crude, the decarbed oil, and the winterized. No delta 10 present whatsoever. So it’s happening in the short path for sure. I just can’t nail down what the catalyst could be.
Indoor or outdoor trim ?
Filtered ventilation if indoor ?
Tour search is for a strong base ! In small amounts
Yust remember
the pfoscheck fire retardant
Creating D10
It was sufficiently present in biomass that was not visually contaminated
My boss thinks the boiling flask temp is too high, but he knows little to nothing about chemistry or short path distillation. I’ve been distilling for nearly 12 years and never had d10 pop at all at similar temps. Super frustrated lol
Who’s carbon scrubbed in that glassware at anytime prior? That’s where I’d look, something has to be chipped and has an amount of a carbon or acidic base carbon. With heat applied this will typically always result in showing a small % of d10 under vacuum conditions. Even a crc is capable of doing this type of isomerization. I wouldn’t recommend it as a good rxn for purpose though.
Now theres an interesting thought…we bought this system used from some hemp boys. Could certainly be the case here. No visual defects present, but doesn’t mean theres something I cant see. I’ll hit up the guys we bought it from and see if they ever used anything extra in the flasks. Excellent idea.
My advice would be to toss some very clean copper scrubby buddies in with your ethanol crude pre-winterization (at benchtop scale of course). Post winterization/filtration proceed as normal.
The copper can bind with free sulphur to form copper sulfides, which are solids and generally insoluble in alkanes, alcohols, and water.
Caveat - My experience with sulphur and copper has nothing at all to do with cannabis, and everything to do with mountain wine, so, take my advice with a grain of salt please!
Boss is a fool temp s you are running are good
Defenatly with all prior steps of clean up
And distilling speed is well within the parameters for clean clean fraqtion cuts
So that is defenatly not the Reading of D10
you need elemental copper in order for that to work; those will have a oxidation layer of copper oxide that will inhibit any absorption and reduce effectiveness tremendously . you can remove the oxide layer with nitric acid or similar strong acid; or just order elemental copper distillation mesh; which will arrive vacuum sealed or elemental copper screens; or shavings/powder from sigma or similar chemical supplier.
Seems to me there are three places to look and eliminate one by one until you find the culprit. First would be your biomass, next would be your alcohol and ultimately your butane. Since you’re using nothing else there’s nothing else it can be… Unless someone in your lab decided to clean glassware/equipment with some chems you’re unaware of and didn’t do a good job of it.
Back in 2019 we had a customer having a weird D10 detection as well. We were seeing a red/rust layer that was forming inside the evaporator. We originally thought our evaporator column was leaking steam into the tube side. Once we got the evaporator column back and pressure tested it, it was fine.
After having the residue tested it seemed to come from a fire repellent that was being aerial sprayed in California.
It has to be something on the biomass causing the issue.
I’m also in camp of small amounts of fire retardant on plants or contaminant in glassware/machinery. I’ve never seen d10 from sulfured plants, but I can’t discount the possibility either.
But i echo the fire retardant stuff; the whole legend about the “discovery” of d10 in the modern rec industry was growers who were distilling material that got hit with fire retardants(phos-chek) when fires hit humbolt in the early days, and had disty exhibiting werid precipitation and crystallization; actually a classic story to tell around the campfire to younger/newer industry folk and chemists alike.
Phoschech is one name for that stuff the plane drops. It was on the biomass that ive had pop hot for d10 in the 5% to 10% range. but high d10 % is from a hoffman reaction. Ive never seen d10 from sulfur but potassium tert butoxide is a good synthe route.
