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Zenochem

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Everything posted by Zenochem

  1. Di-ethyl Ether Gas Scrubbing This might have been covered but I have had little luck in searching for an effective Diethyl Ether gas scrubber. I am about to perform a Di-Ether purification from Heptane using fractional distilling in a Vigreux column (20cm) on a 1.5L scale (6x250mL per my glassware). My problem is that even though this is being performed in a decent fume hood, I have always had significant ether gas drop down out of the hood. This is a homemade hood mind you, however, if possible, I would like to run the sealed apparatus through several gas washing bottles to eliminate ether to air exposure. My first bottle is 700mL with around 200~g of drierite to prevent water uptake into the distillation apparatus on vacuum uptake of atm. on cool-down that I use as a general assembly for anhydrous (or close) distillations. I have two additional 150mL gas washing bottles that can be filled with most common lab reagents except mercury as I do not have enough to fill even a small wash bottle. The water uptake of ether is too small as I have already tried this, and yes, I will continue my own research and DO NOT expect to be spoon fed, however, if anyone has done this before and has a ready answer to the best absorbent for ether fumes it would help. I have spent at least a few hours researching this issue but other than long articles, or my own ineptitude I have not found much that would (in at least 2 washes, 3 tops) scrub the ether vapors to at least 80% efficiency. Thanks to anyone with help, while the vapors aren't an issue for explosive content for the most part for spark proof equipment, fire is always an issue when distilling ether, and I do have all the safety equipment available for a full blown lab fire, as well as personal safety equipment. After a bit more conversation with others we have come to a mineral oil + vegetable oil = atmosphere scrubber system. If anyone has better solvents than this (heptane is out obviously as if I had that I would have never published the question
  2. Zenochem

    Keck Clips

    No, definitely not the wrong size, 19/22 on 19/22 glassware. Much just be crap quality plastics as even the ones on the cold end of the apparatus are splitting, both top and bottom rings. I'll break down and put enough money on some name brand ones, that should solve my issue. I wish I could understand why metal Keck's are in the $50 range for 5 of them, seems incredibly overpriced to me, even for laboratory ware which is always steep on the wallet.
  3. Zenochem

    Keck Clips

    I have purchased two different sets of Keck clips from eBay with average prices of around $1 a clip. Within about a week of use, almost off of the clamps have splits/cracks in them. I am very careful with installation/removal, supporting both upper and lower portions, probably more so than most since I only recently stocked the home lab with ground glass. Running on 19/22 ST joints, which are tight and greased and apparatus is clamped securely with no flexing/etc. to put strain on joints. What (if anything) am I doing wrong, or did I get bum/cheap sets of clips? Anyone else have these issues? Thanks for any input.
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