Hey everyone, we have had some issues (or we think it’s an issue) with some of the winterized, decarbed crude we ran solidified after a while in the 55gal drum. The consistency of the crystallized crude is that of table sugar. The crude oil was cryo-ethanol extracted, filtered through progressive filtration down to .3 micron, solvent recovery auto-vap, then decarbed under vacuum to 133 degrees celsius. During the solvent recovery and decarb we noticed some crystallized solids in the oil and stuck to the sides of the equipment, again the consistency of table sugar and what we are assuming is sugars making it through the filtration.
We had to refund and make right on an order with a client due to this issue as it was not able to be run through their distillation equipment. However, we were able to heat it and run like normal through SPD and achieve very nice distillate and eventually isolate.
Is this possibly due to sugars, or is this crystallization of the cbd due to nucleation from the solids in the heated oil?
Now to make the situation even more confusing, we received some crude oil (extracted from Lifter) from another lab that solidified in the same manner. We have processed a lot of crude in here and haven’t really been able to find any rhyme or reason as to why this is happening.
Any insight would be much appreciated and I am more than happy to provide more info if necessary.
OMG … you have issues, big issues… there must be some things you are missing out. 1st… if this is crude… and half your assumptions are right then it should melt… which it did… and you ran it… so… that appears normal BUT crystallization at these temps and at that LOW potency means something is no Bueno with that oil.
You are sure YOU extracted this??? Yourself?? In Ethanol?
Crystallization will occur over 60% CBD but aggressively over 70%… this does NOT look like crystallization to me, not like this, not uniform like this. It looks like the PH is off on this… and that maybe you used DE during winterization. How did you winterize?
If you noticed crystals during decarb that is … a bad sign… it just shouldn’t happen… not at decarb temps even under vac… at 133C isolate should melt… there should be no crystals… not unless you really have a PH problem or contamination.
Storage temps??? Any other solvents present??? It’s possible at low temps in storage or shipment and with some solvent left in the oil (and a PH that is off) you can get a lava rock effect… kinda looks like this.
Thanks for the reply man, yes we extracted this. I am one of the four people who run the lab equipment. This was consistent with all the crude that came from this particular biomass.
We winterize with -50c ethanol, and then it runs through progressive filtration; 25micron > 5 micron > .35 micron. The 25 and 5 micron are filter socks, and the .35 micron is a lenticular filter (SupraDISC II Lenticular Module (16 in, Flat Gasket) Item No. SD216C).
The finished oil is kept indoors at 74 degrees fahrenheit, no other solvents are used (ethanol denatured with 5% heptane.).
I figured we stumbled across the next big thing, “Crude Oil Crystallate” lol. The product you never knew you needed.
I would start by taking some oil and dissolving into heptane. For example 5 grams oil into 20g heptane. If it’s sugars you’re dealing with it shouldn’t all dissolve in heptane.
Could the material you got from this source be already run material? That seems like a low cbd potency for all the work you did to it
No it was milled here in-house, it was low potency to start with (I think around 5% cbd), long story short, we were told it was considerably more potent. This was some of the lowest potency oil we’ve run through our equipment.
Thanks Alex, I will try that tomorrow. I had tried filtering the hot crude on one of the last batches I did of that through a piece of 30micron mesh, and it pulled out a lot of crap. It looked like charred sugar crystals.
Yeah… was not joking about that… what Alex is talking about is the Hexane brine wash but that gets rid of the “black goo” which is a whole different issue and if you had that in your oil you would know it cause you would not have been able to distill it, it would have ended up as a solid shiny black mass in your glassware. If it is sugars, just wash with water and salt, sugars will dissolve in this. Or you can go the whole hog, and go an Ethanol/Water/Brine wash and see what precipitates. At that LOW of a potency nothing should crystalize. Hmmmm… hey I did see something like this once. When a heat exchanger was damaged and leaking heat (or cold) transfer fluid into the Ethanol extraction system. Check to see if your coolent/heat transfer fluids are missing any volume.
So to do a brine wash, do I mix water and salt, heat, then mix with the crude? Would I then throw back in the decarb to boil off the remaining water? I’ve never done a sort of a water mixture or rinse on oil.
Then mix… mix… let sit for hours and separate then use your reactor as a sep funnel and pour off the shit on the bottom with the water/brine and keep the Hexane/Cannabinoids and then roto the hexane and get your oil back. See what ends up in the water and if there is a funky layer between the oil and the water
Gotcha, I will have to get my hands on some Hexane, we only have Heptane and Ethanol in house. That and I’ll have to see if the boss man wants to even mess around that much with this. I will definitely post any pictures and results from these tests as they are performed.
search LLE techniques and you will find everything you need. its a very simple process and sounds a lot more complicated than it is. just take some of your crude and play around with it in small quantities to get your head wrapped around the process and to see the results before trying on the whole batch.
what temp do you extract at? you say cryo, but what temp exactly? What is the warmest that the ethanol gets during the extraction process? My bet is you’re pulling a bunch of sugars, which the client is correct, would seriously mess up some distillation equipment. If it dissolves in HOT water, you’ve extracted unwanted sugars. Keep that extraction temp cold to avoid it in the future.
