Crystals forming in distillate

[greenXlabs]

Hey guys, I’ve been reading on this forum for past year and gained a lot of knowledge. Now that I am up and running and finally operational after many months of going through the licensing process I came across with a problem that I’m having a hard time resolving it.

I use CO2 extraction method, then winterization with 5:1 200 proof ethanol in -35C for 24 hours followed by filtration with 2.5 micron paper and then roto-vap as usual. After goes the decarbing on a stir plate at 110C for 110 mins. The last step is the distillation for which I use Lab Society’s 5L SPD.

After all this steps I’m getting a pretty good looking distillate at around 75-80% THC content. However, after storing the distillate under room temp in a jar for a day or two a crystallization start to appear. Photos below:

The first time this appeared I reran the winterization process, refiltered with 2.5 micron paper, roto-vaped, redistilled and the result is the images above.

I have another batch that’s pretty similar to this. Any thoughts, comments or suggestions would be highly appreciated.

[IsolationChamberLab]

Sorry to say but if that’s thc distillate then it’s certainly not crystallizing.

Maybe if it was cbd distillate it would crystalize but thc distillate doesn’t crystalize since it’s been decarbed.

What you have is improperly winterized distillate, those are fats/waxes.

Your winterization procedure is off, you really need to go 10:1 with ethanol and get down to at least to -40c bare minimum. You really should be winterizating around -60c to -80c ideally.

It sounds like are using food grade ethanol since you mentioned 200 proof which is good, just a heads up ethanol denatured with heptane won’t get a full winterization though.

[mellodee]

You are not filtering your crude properly. You dont necessarily need cold temps. You just need the right layering.your distillation SOP may need tweaking. You can remove your lipids and waxes during distillation. You can also decarb at distillation under high vacuum which can help dwell times removing unwanted material. Their is another step in post processing we do that removes anything we couldn’t catch before 2nd distillation.

[FreeReggie]

Unless we’re all wrong and he got sold cbd trim

[Hansel]

Edit, I misread your post.

But I doubt he got sold cbd trim if he is buying metric

Could be wrong though…

[RedundantAlexithymia]

when i have seen cbd crash out it the morphology of the solids looked entirely different, then again I am not the most experienced here

[spdking]

1. Might be preprocessing.

2. Might be cbd.

3 . Might be heavy sugars and this needing water wash.

[Demontrich]

Put jar in fridge for a day. If it crystallizes, its cbd. And you got the ole switch-a-roo.

Below is some cbd disty

[greenXlabs]

Guys, thanks for the responses.

@Hansel you are right, I bought the trim from a distributor via metrc. The lab results from the seller showed high THC and almost non existent CBD, so CBD is not an option in this case. I also had the oil tested after extraction at our local test lab which confirmed that there is almost no CBD in the oil.

As for the SPD, @mellodee, let me give you an idea of how I run it.

I start with a small amount of filtered, decarbed crude, at around 200g as I’m still at my R&D stage. I preheat the oil to 80c and then poor it into the boiling flask (which is also preheat). I set the first setpoint to 120C and from their increase the temps slowly and gradually till I hit 200c. Below is the graph of the whole process:

x-axis: time in minutes
y-axis: value (temps, pressure in mTorr)
Red: temp in boiling flask
Lime Green: head temp (vapes)
Blue and Pink: the pressure sensors

So @mellodee, do you notice any spots in SPD procedure that would require some tweaking? Also, what do you mean by “You just need the right layering” ?

And here is another one from couple days ago. This is after the 1st pass distillation. After 2 days I can see some crystal like stuff forming on the surface of the oil and nothing under as you guys can see in the photos below:

Any help is greatly appreciated guys. I’m in the dark with this right, trying to sort this out before I get into my production.

One of you guys said the right words, “…if you ask 10 people about one thing you will have 10 totally different versions to solve that problem.”. So my SOP was structured on 10:1 dilution with 200 proof food grade ethanol, then 24 hours at -40c. And then I was told by a reputable manufacturer that you need more than 10:1 for the ethanol to be able to dilute the crude and separate the bad stuff (waxes, lipids, fats etc). Then another manufacturer recommended to go all the way down to 5:1 and that is the sweet spot for the dilution, and said that with higher ratio the ethanol will bind up with the waxes and lipids and pass through the pores of the filter paper, hence the bad stuff will end up in my oil and not on the paper.

So at this point I’m going back to my initial plan of 10:1 ratio and see how it goes. And again guys, if you have any thoughts or suggestions please share and help me to resolve this problem.

Thanks.

[Demontrich]

Those are sugars on your bf.
2nd pic in the above post

[greenXlabs]

Thanks @Demontrich. Could you let me know how to wash out the sugars? I couldn’t find any info by searching here.

By the way, the flask in the picture is a collection flask and not the boiling, I just haven’t transferred the distillate into a jar yet.

@spdking, you also mentioned this could be sugar related. Would you have any suggestions of how to get read of those nasty molecules?

[spdking]

Warm water washes

[greenXlabs]

By the way, forgot to mention. I also use vacuum grease at the joints, however I’m fully aware of the contamination issue and make sure I use a very small amount of it. At the end of the cycle it doesn’t even pass the half of the neck and I make sure to clean it inside out before transferring the oil out of that flask.

[greenXlabs]

Are there any specific steps I should follow to accomplish this task? And what will I need to use in terms of solubles?

As a preventative measure, what should I do or don’t do to prevent the sugars to end up in the distillate?

[Concentrated_humbold]

Your gonna most likely get more waxes since your running co2, i would no matter the extraction process always filter down to 1 micron. Also up you ratio of ethanol to crude.

[HeisenbergInd]

Use distillate on your joints. Seals better and no contamination.

[greenXlabs]

@HeisenbergInd, ordered couple of these, wanted to give it a try before switching to distillate.

[HeisenbergInd]

We just always used disty because it was readily available.

Never used or tried anything else since so can’t comment on your remedy

[Thetetraguy]

First couple of pics look like fats forming

[ky_cbd]

@greenXlabs I would get her down to a one micron filter when winterizing. I also like to do 10:1 when winterizing.

What does your filtration setup look like? Are you using those round filter papers? What kind of buncher? If the paper doesn’t fit correctly you could be having waxes pass right around the outside of it