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Vacuum distillation advice for a non-chemist?

  1. Jan 11, 2014 #1
    I'm a home-scale experimenter/dabbler in the arts of distilling liqueurs/spirits and essential oils, and right now I'm trying to see what vaccuum distillation(at very low temperatures) can add to the finished product as far as taste, aroma, and color go. For my initial experiments, I've been using a simple glass set-up with a 1000ml boiling flask in a sand bath with a liebig condenser. I've been using an automotive vacuum(for brake lines, etc.) attached to the vacuum take-off valve. I've just been trying to bring ethyl alcohol(everclear) over as an experiment, but I've been having some trouble.

    I'm hoping this thread can be used to troubleshoot some of the problems I've been having and/or correct some of the goofy non-chemist methods i may have been using from the start.

    Right now my biggest problem is that I seem to be losing vacuum. This may be through one of the clamped connections between where the glass fits together, or it may be from the tubing connected to the vacuum take-off. Is there a good method to check for leaks or a fool-proof method for sealing connections so they can't possibly leak in the first place?

    Here are some pictures:


    I have been using vacuum grease with ground glass joints(+keck clamps) that fit well together, so I'm doubting that I'm losing vacuum through the actual glass connections in the set-up, although I'm still entertaining that possibility.

    My thought is that I'm losing it through the tubing I've attached to the vacuum take-off. I used a flour-based paste to seal it over, but maybe that isn't the best idea? Maybe the tubing itself is too porous and I need to get higher quality tubing? Any idea as to resources to find this?

    Also, if anyone wants to throw any critiques out there about the set-up I'm using(after viewing the pics), I'm all ears. I'm totally a novice and I'm sure I'm making a lot of stupid mistakes that I'm unaware of.

  2. jcsd
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