Filtration under inert atmosphere technique | Tetrakistriphenylphosphinepalladium treating

We hit 500 subs 💗!! Special video soon! Thank you very much! Let's go for 1K :^) As I promised, showcase of my filtering system for Tetrakis " Pd[PPh3]4 " _ - FULL TEXT - _ First of all, I have prepared a fresh portion of tetrakis in DMSO. I used a Schlenk flask as before. Next, we should prepare T-shape outlet by greasing its taps. I highly recommend Dow Corning vacuum grease, this lube isn’t expensive and pretty robust as well! Taps are linked with a backbone via wire because pressure gap between vacuum and argon from balloon or inert gas line, whatever you want, could easily shoot them to the four winds. Outlet contains 14 mm joint equipped with porous glass filtering surface. Other joint must be covered by empty well dried round bottom flask. Further, Schlenk vessel with the reaction mixture is placed into clamp. Now watch carefully. Outlet taps are closed, and now you need to switch on an argon flow. In my case by opening a plug connected to balloon. Next, remove the septum, purge argon a little bit, then seal the construction at all. Now please turn the stand like this, Schlenk flask should be easy to rotate by hand. Vacuum socket of outlet should be perpendicular to the argon entry. I am gonna use a water circulate vacuum pump. Ok! Let’s go to start. Open a vacuum exit tap, connect a pump hose, then turn a hole construction upside-down, shaking well a reaction mixture in the main flask. Now open an argon flow and the middle tap. Nice! As you can see, DMSO with impurities starts to move out the Schlenk flask. When tetrakis precipitate is filtered off just disconnect a vacuum in reverse order to previous procedure. Receiver vessel should be removed and washed by acetone. I do it to ease purification stages check with UV-light. Because impurities have more yellowish color of fluorescence than desired product. The next step is washing tetrakis with methanol, three time 15 ml portion each. For doing this, seal an argon tap, remove a balloon. Further take a portion of methanol using syringe BUT don’t forget to let air bubbles gone out. Hey, don’t forget to get balloon back! Now put the point of injector into hose like this, and push liquid simultaneously opening the tap. Next step is just a reverse version of previous one. Before doing the same with diethyl ether, don’t forget to use a clip cuz this solvent gives a huge pressure difference due to its extreme volatility under vacuum. This step is overlong because of frosting and crystallization in the middle tap. Of course you should do it three times 15 ml portion each. After all washing routines, I just cover the workspace with paper sheets and put tetrakis into weighed bottles as quick as possible. As the result 2.750 grams of pure product, around 87% yield. Nice! Finally, just seal vials into a bigger glass vessel flushed with argon. -------------------------------------------------------------------- Socials: ► Support me on PayPal: https://paypal.me/acantharex Music: 1) Part Native & Oly - Artificial Love [NCS Release] 2) T & Sugah ft. Mara Necia - Bring Me The Light (Rob Gasser Remix) [NCS Release] -------------------------------------------------------------------- Tags: #organicchemistry #argon #acantharex #inorganicchemistry chemistry, organic chemistry, guide, tutorial, experiment, fluorescence, solid state, evaporation, inorganic chemistry, laboratory equipment, science, routine procedures, how to, palladium metal, argon, nitrogen