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Oct 17

Inquiring Minds Need Your Help

by Kenneth Hanson | Categories: fun, Uncategorized | (113099 Views)

My current adviser has successfully managed a research group for more than 30 years. He has produced hundreds of publications and acquired a wealth of chemistry knowledge. Last week, when the group moved into a new lab, we boxed and unboxed the tools that helped build this knowledge: a grand collection of equipment, glassware and chemicals.

It has become abundantly clear that with much knowledge comes much glassware.

And not simply your everyday beakers or Erlenmeyer flasks, but unique glassware created for specific experiments. While this glassware once had high utility, it is now a fossil of long-ago projects gathering dust in the archives (and by archives I mean that drawer full of weird glassware that no one uses).

The graduate student or postdoc who preformed the long-forgotten experiment has moved on and taken with them the explanation of the glassware’s function.

The inquiring minds of my research group would like your help in identifying/explaining the five of the most interesting specimens.

1) The Immersion Condenser
The first item is an immersion condenser or cold finger with an o-ring connector and an inlet/outlet for cold water. The question is why does it have the weird tip at the end?


Since many of you are currently trying your hardest to come up with a funny/witty comment, I will make a preemptive, unclever strike: PENIS! PENIS! PENIS!

2) The Pitch Fork
Each of the glass rods in this image has a small (~1-2 mm) tube inside so it behaves as a four-way junction. Why this specific shape?

3) The Meth Pipe
This item has two openings. The smaller one has a long stem that encircles the larger opening several times until they both meet in a conical chamber. As you can tell from my label, our guesses on this glassware’s purpose were limited.

4) The all-in-one Reflux/Distillation/Addition Funnel Apparatus
The form of this item is relatively straight forward with the exception of the absent Teflon or glass stopcock just above the lowest round bottom flask. What is it for?

5) The Bubbler
This is the piece that I am most curious about. At first glance it appears to be a plain bubbler with a smaller inlet tube that runs to the bottom of the larger chamber which has an outlet near the top. Upon further inspection, we find that there is an additional, independent piece of glass in the inner tube that is free to move vertically (inset). The independent piece of glass is a sealed chamber either filled with a gas or is simply a vacuum. On the top of this piece is a ground-glass ball joint. The counter to this ball joint is a socket with an opening from the top inlet. Our best guess for this piece is that, unlike a normal bubbler, the inlet is reversed and is for liquid to flow directly into the larger chamber. As that chamber fills, the freely moving piece is buoyant and will continue to move upward with the solvent. Once the chamber has filled with enough solvent it will push the ball and socket joint together preventing the further flow of liquid. If this guess is indeed correct, what would you use it for?

Any insight you can offer is greatly appreciated.

15 comments

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  1. Dave

    1) No idea, how does the water circulation work in the end of the piece?
    2) My first thought was that it was the end of some kind of mechanical stirrer, but that doesn’t really make sense at all…
    3) possibly the receiver for some sort of distillation apparatus. Air cools in the long tube, removed from the straight tube.
    4) A permanent still for something very sensitive. Keep it in the back of your hood, with a drying agent or what not in the bottom, fire it up when you need it, remove the pure liquid from the top and then drop the rest back into the distillation pot for next time. Boom.
    5) I agree with your guess. Might be useful for some sort of a larger scale reactor that might produce back pressure on a line. This would prevent reverse flow. Just a guess.

  2. KNP

    Well, the first peace looks alot like a sublimation apparatus (although I’m use to them with a vacuum adapter on top). http://quarkglass.thomasnet.com/viewitems/sublimation-apparatus/qsu-2-sublimator-vacuum?

    The last one looks like Lafler Bubbler. It can be used to control the pressure in your manifold line. You add oil to the reservoir.
    http://www.chemglass.com/product_view.asp?pnr=AF-0512

    For the second one… looks like someone just got fancy with the blow torch and some glassrods… 🙂

  3. Big Bad Chem Daddy

    1st one has gotta be a top to a sublimator–I bet the shape is to give you more surface area right above the crude material, where most of the crystals tend to form. With the flat-bottomed ones, I’ve seen crystals regularly break off and fall back into the crude mixture. If only I had one like that two years ago. Still, the bottom would have to have the vacuum outlet, which I can imagine might be a pain in the butt.

    I bet 4 is for doing distillations of small amounts of reagent-type things (TiCl4, for example).

    The others just look like a glassblower got bored.

  4. Steve

    My first impression on the bubbler is that its a neat way to prevent ‘sucking back’ the contents of the bubbler.

  5. Chris

    As far as the pitchfork shaped one goes, maybe a way to sparge the reaction solvent and stir it mechanically at the same time?

  6. mitch

    4) Definitely looks like a small-prep solvent distillation setup.

  7. Bryan

    I’ve used the bubbler before and I agree with Steve that it’s used on vacuum manifolds to prevent suck-back of oil. My old group did not use mercury bubblers and instead used those.

  8. cookingwithsolvents

    1) could be used for sublimation but likely for distilling v. v. small quantities of air-sensitive liquids. Using a long tube allows you to immerse most of the apparatus into the heating oil for v. high-boiling stuff (similar to Kugelrohr but the clamp means you can bring it into a box to get your stuff). I’ve used a very, very similar setup.

    2) I see multi-junction and think e-chem but I have no clue.

    3) slow addition of viscous liquid with a slow gas flow? actual pipe?

    4) I concur with mitch: small still (perhaps for a reagent rather than solvent, what is the volume?)

    5) yup, bubbler w/ check valve to prevent back pressure when venting gas (e.g. HCl evolution when making a metal alkoxide from the MClx). you can buy them commercial now.

  9. anon

    #5 is called a Cartsian Diver. It regulates the pressure of a vacuum.

  10. Andrew

    #4 is probably for distilling small quantities of expensive solvents or reagents. I’m thinking of CDCl3, etc. The top of course should be connected to a Schlenk line for pressure relief. Seal the tubing with a septum, run the cooling water, and allow your compound to reflux with your drying agent. Close the tap and start to collect. Once done, transfer out via needle/syringe.

    #5 is to prevent suckback. Put it as the outlet on your argon line. When you backfill an evacuated flask, some silicone oil is sucked up the wrong way. Without a device like this, you will suck it all the way into your Schlenk line, *even if you are very careful*, simply because silicone oil isn’t very dense. I suppose a mercury bubbler won’t do that, but most people use silicone.

  11. Chad Brouwer

    #1 is definitely a micro-distillation apparatus. Actually, it is only the top half. The bottom half would be similar to a sublimation apparatus’ bottom half. The liquid to be distilled condenses on the ‘shaft’ and runs down into the collection ‘head’, if you will, where it can be collected with a pipet.

  12. osmium

    I’m an electrochemist, and when I saw #2 I also thought it might be something electrochemical. I have NO IDEA WHY you would need this, but it could be like a Luggin capillary that goes to 3 locations.

  13. P.J. Rafter

    The topmost piece might benefit from increased girth – well, the recipient certainly would, then!
    Alternating hot and cold water circulating in the “thing” might have intriguing possibilities . . .

  14. David Crabtree

    From the size of the chamber at the intersection on the pitch fork I wonder if it may be used to mix three different reagents together by applying a vacuum at the other end? Then IR or UV/Vis the mixture between the two blobs of glass at the end? If that’s true, though, I don’t see why the forks point together instead of away from one another? Does it fit nicely on a three-necked RB flask?

  15. Labchimp

    No. 3 I have used before. It can be used to condense volatile liquids exiting a preparative gas chromatograph. You just submerge it in ice water or dry ice etc.

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