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How to perform a vacuum sublimation | Quick guide скачать в хорошем качестве

How to perform a vacuum sublimation | Quick guide 3 года назад

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How to perform a vacuum sublimation | Quick guide
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How to perform a vacuum sublimation | Quick guide

Hello everyone! Today I'll show you a quick guide dat help you to perform a vacuum sublomation! :D FULL TEXT First of all, you need sublimation apparatus, for simplicity I’ll call it sublimator. This is an apparatus base. Oh yea before starting all of procedures, you should cover the workspace using some paper sheets. To move your initial material into sublimator I recommend to make a paper tube to prevent mid from contamination. For today’s experiment I am gonna use sample of dried slurry after Suzuki-Miyara coupling reaction. Good I put the whole stuff in apparatus and now you need to grease core joint a little bit but isn’t higher than half of inch. It’s essential because if you use a vacuum, sublimator could stuck really hard. So, do not use too much lube! Correctly greased joints should be transparent along the perimeter. The excess of lube could be removed by a glass stick. Further we need a thermos of liquid nitrogen for trap which prevent a vacuum pump from moisture and fumes. Now let’s go to set up a whole construction! For heating I’ll use a Wood’s metal in the steel cup. Put the apparatus in clamp then connect water hoses so that water circulates top down. Ok, we are ready! Now put down a trap vessel into a liquid nitrogen and just turn on the vacuum pump. Obviously, don’t forget to put sublimator into Wood’s alloy, that would be really sad to forget about that step 😊 If you want to perform a fractional sublimation, it’s necessary to install a thermometer into heating bath. Hey, be gentle with liquid nitrogen and wrap it with a little towel. How does fractional sublimation work? Simply! Compound is heating to its sublimation point and turn into gaseous phase. Vacuum helps you to decrease this temperature. Then vapor just cool down on the sock chilling with water, producing crytals of purified solid. Different molecules have a different sublimation temperature so you could isolate them from each other. For this method, successful separation is achieved with a phase temperature difference of at least 10°C. Now I propose you to take a look at small time-lapse of crystallization process. Yep, my stuff has a nice blue fluorescence. After sublimation process is gone remove the thermometer and put off a sublimator from bath and let it cool down. Further, remove whole Wood’s alloy from it I’ll use an used Silufol sheet. In general, we disassemble the installation in the reverse order of assembly. Clean product could be collected from sock using scalpel onto metal or paper surface. I highly recommend you to use funnel and boat from aluminum foil to prevent content from electrification. Vacuum grease cleans well with n-hexane! As you can see I have collected a small portion of nice and clean dye. -------------------------------------------------------------------- Socials: ► Support me on PayPal: https://paypal.me/acantharex Music: 1) Arcando - In My Head (feat. Britt Lari) [NCS Release] 2) Chris Later & Dany Yeager - There's Nobody Else [NCS Release] -------------------------------------------------------------------- Tags: #chemistry #vacuum #sublimation #guide #science #acantharex chemistry, organic chemistry, wood's alloy, wood's metal, sublimation, vacuum sublimation, guide, tutorial, experiment, fluorescence, solid state, evaporation, inorganic chemistry, grease, laboratory equipment, science, routine procedures, fractional sublimation, fractional distillation, aluminum foil, lube, scalpel, how to, hexane

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