Oil Drops in Distillate?

Hey Everyone,

I need some help.

Recently started making distillate. This site has been extremely helpful. So thank you everyone for contributing.

I have an issue I haven’t been able to find any solid answers to. Hoping someone has experienced this before.

I have what appears to be oil droplets/bubbles in my distillate. At first I thought they were air bubbles, but on closer examination I realized that it was oil. (Picture at bottom of post)

Now I see that all my crude from this batch of biomass, has small oil specks floating on top, and the consistency is kind of runny (this is post winterization). I speculate that the material was sprayed with some kind of vegetable or petroleum oil based pesticide. Considering the results (see pic) does this sound plausible?

I have done some searching around the forum and haven’t found any definitive answers to this problem. Here is the information I have found:

@ScoobyDoobie posted the following in

In both cases i just dissolved the extracts in hexane, chilled with dry ice and filtered the solution… Followed by brine washes. Green cleaner was harder to remove due to the goddamn sodium laureth sulfate…

Scooby also posted this

Green cleaner is primarily made up of sodium lareth sulfate and soybean oil which would be easy enough to remove it from an extract solution with the addition of potassium hydroxide to react with the soy ran oil followed by mixing with attapulgite clay for subsequent filtration.

I don’t know if I am following this correctly, but it sounds like: dissolve oleo in non polar solvent and do a brine wash with a high enough pH to saponify the vegetable/petroleum oil?

So then I searched saponify and found the following from @Future and @Photon_noir:

These triglycerides, we can saponify them with alkali and wash them out when doing a saline scrub, right?

@Future Nah, saponification is probably something you want to avoid, since that would cause your cannabinoids to be micelle-soluble in polar solvents like water… and conditions that caustic should be avoided for other chemical reasons.

The above leads me to believe a high pH brine wash is not the right tool for the job.

I also found these bits of gold from Photon referencing MgO in response to a question posted by Square Root:

I have not left it in for any WFE processes. It can be partitioned into water from non-polar solution of the crude, which also helps saponify and wash out vegetable oils… oops! I let another hint slip! :wink:

Understand that saponification is the creation of soap, a strong emulsifying agent, from fatty acids. That means partitioning non-polar resin solution with water can cause issues with the partition. It helps to use fairly briny salt water for the first wash or two.

Also know that the heat processing of the oleoresin causes oils to break down into smaller chains of more similar sizes. This actually could be beneficial,sincethe soaps would be more water soluble and less non-polar (cannabinoids, but not necessarily the solvent) emulsifying.

So I am starting to think: dissolve first pass in 1:1 (?) heptane add MgO (<=5mL per 1000g of oleo) to oleo/heptane solution. Mix at high temp (?) for 20 to 30 minutes. Add saturated brine solution, agitate, allow to seperate and filter. Repeat until water comes off clear. Wash with DI water to remove any remain MgO. Do I need to worry about the pH of MgO? Recover heptane. Second pass.

Edit: Maybe add the MgO dry so more heat can be applied? Then dissolve in Heptane and wash?

Any insight on either of these processes would be greatly appreciated, or just a wink and a nod if I am on the right track.

Thanks Everyone

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I suggest you dissolve the crude in methanol and chill with dry ice. This does a good job of removing most of the components of vegetable oil. But did you produce the crude? The oil may have been introduced via pump malfunction.

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I tried rewinterizing but just standard freezer temps. I will try with dry ice and post my results.

I produced the crude. I use a rotary vane pump to filter through the buchner so that is a possibility. If that is the case will winterizing at dry ice temps help?

I appreciate your response

Winterizing out light oils like that is very tricky, with hardly any agitation they will dissolve right back into the solution. So the keys to making this work as well as possible go like this.

  1. Use methanol as your solvent, it’s more polar than ethanol so it’s better for this purpose. You will want to try to make the solution as saturated as possible, this will cause more shit to drop out when you chill the solution. I probably used roughly 4:1 ratio of solvent to extract.

  2. Chill the solution with dry ice and allow the precipitates to drop out, with something like vegetable oil it just makes your solution get very foggy so if you have bentonite it helps to cause the precipitates to form into a floc and allows it all to drop to the bottom of the solution.

  3. Use a taller skinnier vessel to chill the solution in, because when you have a solution that’s that concentrated and that cold you’re going to have a hard time getting it thru a filter. So the idea is to allow whatever preciptates to fall to the bottom of the vessel and then instead of filtering the solution, siphon the solution from the top.

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And if you do have reason to believe the oil came from a pesticide then you should still perform some ph swing brine washes because those pesticides usually have other shit in them like emulsifiers and the like.

It would be obvious to you if you accidentally sucked oil from your pump while you were filtering, I dont think that’s the culprit.

Maybe the material went thru an auto trimmer and soaked up some oil somehow?

Also you will likely have some isomerization issues when heating in the presence of magnesium oxide.

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Thanks for the detailed replies, very helpful.

I usually leave my buchner unattended because it takes a long time and I filter inside a freezer so id have to open the freezer to look anyway. I don’t think that is what happened but it is a possibility and I have no way to know for sure.

It was machine trimmed so that is a possibility as well.

If it’s a synthetic oil that was used to lubricate the trimmer then sadly I got no advice for you :frowning:

Doesnt mean it cant be remediated or anything, I just dont personally know.

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I got a few things to try. We’ll see how it goes.

Just heard back from the supplier, he claims that the person that got the other half of that batch of trim had no issues and he sent a pic. No reason to doubt him. So it must be on my end. Either a vacuum issue I didn’t notice. Or some kind of vegetable oil from the 55 gallon drums i used for bucket tek. I added new drums this run, the drums were used but cleaned at a professional facility and I wiped them out quickly with acetone, but they seemed very clean so I didn’t go in as hard on them as with the first batch I got. Seems highly unlikely but impossible. Those are the only two things I can think of, either way I won’t let happen again.

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How do you know that it’s an oil?
Are you positive it’s not water drops?
I would think that if it was oil and the distillate comes off the still warm that those two would mix, water drops would stay separate.

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If you didnt close off the vac pump while the spd was under vac, and you cracked say a gl fitting to break vac, you sucked vac oil/vapors into your disty 100%.

Qhen you broke vac, that spot is equaling out the pressure from anywhere it can, even your vac pump.

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I don’t think water vapors would condense at temperatures and pressures present during distillation. But I do not know for certain.

Edit: Have you experienced water dropplets in your distillate before?

I haven’t broken vac on the spd without isolating the pump. So I don’t think that is the culprit. But I think that is exactly what happened with my buchner funnel. I shut off the pump without isolating it. Didn’t see any backflow. But the cake I used was thicker than usual, so i am guessing there was more negative pressure and some oil got sucked back in. That seems the most plausible answer.

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I only know this from experience. I did this when running my cav oven I didn’t close off the vac pump and it sucked oil right into my vac oven

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Haha I’ve done that too. Should have known better. But when your starting out with budget equipment and running around trying to get everything done yesterday, things slip through the cracks. I’m sure you can relate. The past month has been one continual lesson in slowing down and doing things the right way every time. Not that I didn’t already know that, but I guess I’m a glutton for punishment. Appreciate the response

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Water would almost certainly be on the bottom, is heavier than hemp/can oils

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The bubbles dont want to move up or down when heated and agitated.
I heard that crude was around ~.9g/ml and distillate was ~1.1g/ml. Haven’t measured it myself, but I know I can fit 500g of distillate in a 16oz mason jar, which leads me to believe it is atleast a little heavier than water. I’m guessing your experience differs. Have you calculated the density of distillate? I’m curious to know what your getting.

Yeah I was thinking crude , should have read post title better lol. I haven’t measured distillate density and sounds like you have. I’m pretty sure I’ve seen crudr be heavier than water even so, maybe it’s water on your distilate? See if it mixes with water

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I’m sure things can vary quite a bit. I will test and see. I appreciate your input

Hi there,

this is actually my first comment after weeks of lurking in the shadows.

Ive had a theory about these oil bubbles, at first I thought it might have gotten sucked in somehow from my rotos trivac but after closely monitoring I had to rule it out.

I think it might be coming from the dry ice we’re using.
I also extract with dry ice and I feel like whatever blades they use the cut the ice into nuggets might be getting into my material but to be honest, I have yet to reach out to our various dry ice companies to ask, however I have noticed the oil comes up less when we use dry ice in the form of blocks.

I guess it also has to do with how these companies are handling their DI from their end but again, just a theory Ive been working on.

Cheers

Did you ever figure this out?

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