Weird problem

Hash and Stuff Distillation
1

Ok so if any one has time to help on this I would really appreciate it. I am doing distillation R&D for a type 7 in Nor Cal.

I am working on a simple 2L short path with a Welch1400B. The crude came from an 80% propane/20% butane run that was winterized at -40C and decarbed at 85C and 7.6 torr in a vac oven for 3 hours.

Everything was going pretty normal through the heads fraction. Right about 195C at 200-ish microns, when I would normally be expecting cannabinoids to start dancing in the vig, I instead saw my mantle rocket up to over 400C and then read HHH for about 20 secs, before then shooting back down to just above my set temp.

And then… nothing. I inched up the temp 5 deg at a time until I was at 220 and literally nothing was coming over. Good swirl. Vac down around 50 microns. Nothing in the vig. No cannabinoids.

Am I crazy? Is my mantle fucked? It’s as if the entire cannabinoid fraction is missing!

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Since you mentioned the HHH it makes sense to assume your probe is the issue.

  1. Try reading the temp with a replacement probe. A short/loose connection or exposed wire will cause the temp to read HHH.
  2. Try reading the vac directly from the pump without the glass assembled to make sure the micron gauge is accurate.
  3. Do you read vapor temps? Were they still rising along with the flask temp?
  4. Are you certain your mantle is still heating?
  5. Did your cold trap fill with terps and clog the lines?
    Let’s start with those questions.

Wait…did you say the BODY was missing?? Are you saying you have no mass in your receiving flask, boiling flask or cold trap flask??

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  1. Unfortunately I would have to order a replacement but I agree this would be good troubleshooting.

  2. The gauge is good. I changed the pump oil before the distillation and when I placed it directly on the pump it went down to 1 micron and when I took it off it went back to 760 torr.

  3. I do not have the ability to read head temps on this setup.

  4. I know it’s heating enough to keep the crude liquid and bubbling, but that’s all I can say for sure.

  5. Cold trap was good and clear.

Crude was boiling in the bf. Heads were dripping over as normal. Suddenly the heads stopped coming over, the temp shot up, then back down again, and now in the temp/vac range where I should be getting body I get zip zero nadda.

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20200225_124004
20200225_1240044032×3024 3.09 MB

Pic of setup.

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5

Ya its the probe…

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Thank you for the help! Yes, it turned out to be the probe. When the error happened again I jiggered with it just like you would a loose headphone or usb cable and voila… it works now. Just about to hit my mains.

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When you find a place that sells replacement probes for those mantles let us all know where to find them!

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What’s so special about them? I have a hard time believing that what they’re fitted with is anything all that far out of the ordinary, and I’ve got a few different shops that stock or can order a variety of different types of temp probes. If someone in the Denver area has one with temp probe issues LMK I’d be happy to lend a hand.

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I don’t think there’s anything really special about them per say. I haven’t been able to find one with the plug end that mantle uses. They all say they’ll order it. It never shows up. If you have a supplier who has them a link would be appreciated.

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Got a picture of what it looks like?

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I’ll post one up tomorrow when I get to work

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