September 28, 2024, 06:43:11 PM
Forum Rules: Read This Before Posting


Topic: vacuum distillation advice?  (Read 3143 times)

0 Members and 1 Guest are viewing this topic.

Offline cruelwhencomplete

  • Very New Member
  • *
  • Posts: 1
  • Mole Snacks: +0/-0
vacuum distillation advice?
« on: January 11, 2014, 02:38:27 PM »
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 vacuum 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:

 
http://s129.photobucket.com/user/erzulie_tartar/library/lab
 

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.

Thanks!

Offline billnotgatez

  • Global Moderator
  • Sr. Member
  • ***
  • Posts: 4428
  • Mole Snacks: +224/-62
  • Gender: Male
Re: vacuum distillation advice?
« Reply #1 on: January 11, 2014, 08:53:24 PM »
Could you attach the photos of interest directly to this forum
That way we know for sure which photos apply
and
they do not go away in the future due to a bad link occurring

Offline Arkcon

  • Retired Staff
  • Sr. Member
  • *
  • Posts: 7367
  • Mole Snacks: +533/-147
Re: vacuum distillation advice?
« Reply #2 on: January 12, 2014, 09:09:28 AM »
I think this is the most useful picture.
Hey, I'm not judging.  I just like to shoot straight.  I'm a man of science.

Offline billnotgatez

  • Global Moderator
  • Sr. Member
  • ***
  • Posts: 4428
  • Mole Snacks: +224/-62
  • Gender: Male
Re: vacuum distillation advice?
« Reply #3 on: January 12, 2014, 05:32:09 PM »
I would apply a slight pressure to the system and try soapy water spayed on areas of the system you think might be leaking. Where the soapy water bubbles is where the leak is likely to be.
But, I am doing the old leaky tire trick as a part of common practice on tire pin hole leaks. The lab folks here may have another trick.

Offline zoork34

  • Regular Member
  • ***
  • Posts: 47
  • Mole Snacks: +3/-0
Re: vacuum distillation advice?
« Reply #4 on: January 15, 2014, 05:03:16 PM »
Where did you get your ball flask that has ground glass joints on both sides?  I've been looking for one of those. 

Sponsored Links