The ethanol is chilled to -50°c and the warmest it gets through filtration is -25°c.
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That is one key to the problem, 25c isnt cold enough to prevent sugars.
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I second thesk8nmidget!
Interesting, do you have recommendations on what temperature we should hit? Or where I can find information about this?
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You can search here and find a lot of answers but I’m pretty sure the general consensus is -60 is the warmest you wanna Allow your process to reach.
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-67C to stop pulling lipids and chlorophyll. Sugars, though, I’m not entirely sure about. I had no shortage of issues with sugars while extracting -40C to -55C. Stepping up my filtration game was what more or less solved it for me, not getting colder.
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Where’s you get -67 specially at?
@SirWest sugars can be completely unrelated to temp. If your solvent isn’t high enough proof that can be an issue. Over milking the material to powdery can also be an issue.
We can try going colder, but I don’t know that we can get any better filtration. Only hopes and dreams make it through .35 micron.
Hi Siosis, we use 200 proof ethanol, denatured with 5% heptane. This particular oil we have was extracted the same as our other biomass that we had in the building. The strange thing with the sugar conspiracy, is we have had perfectly fine oil come from biomass that was known to have very high sugars from the hemp itself as well as wheat and other plants growing amongst the crop during harvest. That farmers lot came out to be very nice oil, distillate, and isolate.
This one particular lot is the only one we have produced with this issue. At any rate, the R&D beaker for the LLE experiment should arrive today, so I can do some separation and see what results I get.
Did you try to dissolve in heptane or hexane? What was the result?
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Well… hopes , dreams, mold spores, sugars, etc all come through at .35um. I prefer going down to 0.2um, but that is not exactly what I am talking about. You are only filtering two dimensionally. Time to incorporate magic dirt and do three dimensional filtration PLUS the standard 2D filtration down to 0.2um.
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So im very late to here but i think you can help me. I believe i am having the same back goo that turns into shiny solid almost like a plastic when running our 2nd pass on our 4" WFE. The equipment we started with here was the ethos & ares by capna with the WFE. Do you have suggestions on how to prevent the oil from becoming that goo/solid? I would really appreciate the feedback.
This is my answer based solely on my own experience with our WFE. That Black Goo is the “Tails”, heavy, high boiling point compound after you have evaporated the cannabinoids. You can use an additive oil in the process, as long as it too has a high boiling point. I am currently experimenting with canola oil and soybean oil. So far I am seeing really good results, both from a distillate yield standpoint, and the tails are a lot thinner so they slide out of the machine much easier.
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Yes my WFE gets clogged and is difficult to recover any tails in the process at all, some at the end but not much. Most of it comes out only on the wash after the run.
There’s no way you have this much gum contamination but with the convo about sugars I figure this might be an opportune time to mention the way to test if something is a gum: the Acetone Insoluble Material Test.
“Content of acetone-insoluble matter— If the substance under test is stiff, soften the Lecithin by warming it briefly at a temperature not exceeding 60 , and then mix . … Add acetone that previously has been chilled to 0 to 5 to the 40-mL mark on the tube, stirring during the addition.” - wiki:lecithin
The point of all that is that contaminant that doesn’t dissolve in acetone is most likely gums. Sugars dissolve in easy ways as mentioned above.
That is all, cheers.
What’s the shiny solid like when cooled to room temps?
Back when my lab was still doing room temp ethanol extraction we would get those nasty things in our rotos during solvent recovery, and at room temp they were very hard and brittle, and would shatter like glass if dropped once cooled. We no longer had any issues with them after moving to cold extraction.
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It was almost like a brittle plastic in my opinion.