1. In a 2 liter glass flask or beaker put 230 ml of concentrated H2SO4 in litter flask and add magnetic stir bar put into Ice bath of appropriate size allow for acid to cool to 0 C or relatively close ( IE 2 C - 10 C is also ok )
2. Pre –oxidized graphite powder is stirred in slowly to the mix 10g and allowed to fully mix with stir bar.
3. 30 grams KMnO4 Is added to mixture this is done slowly 0.5 gram at a time mixture will rise allow to cool back down before adding another gram AT NO TIME DO YOU ALLOW THE MIXTURE TO GET CLOSE TO 90 C AT 100 C IT BECAUSE POTENTIONLLY EXPLOSIVE MANTIANE AN ICE BUCKET
4. DI water is added (460 ml) Important to not let experiment go unobserved at this time the mixture is stirred at 35 C for 2 h ( WARNING WATER WILLM HEAT UP REATION TO DANGEROUS LEVELS USE AN DROPER TO DROP IN WATER SLOWLY MAINTAIN 30oC )
5. After 15 min stirring the reaction is terminate by addition of large amount of DI water up to 0.7 liters and 30% H2O2 is added (150 ml) the color of the mixture will be bright yellow at this point.
6. Make a HCL wash 1 part Conc. HCL to 10 parts water in a 1 liter beaker pour 150 ml in centrifuge tubes and add 100 ml of Graphite mixture. Balance out centrifuge tubes and spin at high speed for 5 mins
7. Pour off supernatant and add DI water to full and shake mixture in bottle.
8. Place back in centrifuge and spin at high speed for 5 min 30,000 or less ( does not take much speed for separation )
9. Pour off the supernatant in each bottle pour 20 ml of Di water and swill till graphite oxide suspends in solution.
10. Alterative to centrifuging is to pour equal amounts in 1 litter PPE bottles and top off with DI water. Allow to sit over night Pour off supernat.
11. Vacuum filter final solution washing with DI water till PH paper reads neutral.
12. Testing of product can be done several different instruments. The easiest to use is the UV spec you are looking for a peak around 220nm to 230nm and a shoulder at 300-310 nm
Pages in category "Grapite oxdation"
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