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Synthesis of Graphene Oxide by the modified Hummer's method used in the GESMAT group. 

CIGMMAD Colaboration
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This is the detailed synthesis method for Graphene Oxide using the metholodogy reported in our paper:
"Graphene oxide powders with different oxidation degree, prepared by synthesis variations of the Hummers method" published in Materials Chemistry and Physics 153 (2015) 209.
dx.doi.org/10.1...
by J. Guerrero-Contreras and F.Caballero-Briones.
feel free to reproduce and improve the method, please cite us.

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5 сен 2024

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Комментарии : 85   
@cigmmad
@cigmmad Месяц назад
@rosellenunez6363 if It is "brown" seems fine..try to suspend 100 mg in 200 ml of water. It has to be completely dispersed, not settled. Did you dry the product slowly, at low temperature?
@realandimaginedxyz
@realandimaginedxyz 3 месяца назад
I can't easily get HCL, is there a better way to remove Mn ions? Would it be a huge problem to just wash with water to begin with? Would the leftover ions really interfere with GO?
@cigmmad
@cigmmad 3 месяца назад
Well, Mn would induce other effects, such as catalytic Activity, so depends
@realandimaginedxyz
@realandimaginedxyz 3 месяца назад
@@cigmmad I am going to try using it in electrochemistry, primarily for enhancing anodes in batteries in experiments. I wonder if there is any other way of getting rid of Mn.
@yohanatamara1771
@yohanatamara1771 Месяц назад
Hello, after you add deionized water for the second time, how long should you wait to add H2O2 and what temperature should it be at? Another thing when I added the water the second time the solution changed from dark brown to black.. Any advice, as I am trying to get OG from the cashew seed by following these steps, but it is not working.
@user-mj2mh6hk8n
@user-mj2mh6hk8n 6 месяцев назад
Friend, I followed all the steps according to the article but the solution did not turn yellow or brown when adding the DI water together with the hydrogen peroxide
@cigmmad
@cigmmad 5 месяцев назад
Fast addition or KMnO4 during oxidation or if H2O2 and water at ehe end may reduce GO and turn black the suspension
@ridarida3154
@ridarida3154 3 месяца назад
Also plz explain the centrifuge process in you videos of GO and washing. If you don't mind thank .
@cigmmad
@cigmmad 3 месяца назад
After we got the GO solution, we put the solution in the centrifugue tubes, as.many as they fit in the centrífugue machine (6 in our case). We centrífugue, remove the supernatant, add HCl 5%, shake to resuspend some 2 min, centrífugue, and repeat three times with 5% HCl and other 3 with DI H2O. In the latest wash we recover powder with some remaining water in a porcelain capsule to dry in the oven at 60oC by 24 hr ñ.
@atifafroz1821
@atifafroz1821 3 месяца назад
Very demonstration
@rosaliaimroatulmufidah7450
@rosaliaimroatulmufidah7450 2 месяца назад
Hi, I am doing GO synthesis but the final pH after washing with DI water is still acidic. Should the pH of GO be neutral and is there a pH requirement that must be achieved before the oven? thank you.
@cigmmad
@cigmmad 2 месяца назад
@@rosaliaimroatulmufidah7450 hello, yes, it is normal. The washings with DI water after HCl are intended to remove Cl ions. But pH of a GO suspensión is around 3-5, normally. Best regards
@rosaliaimroatulmufidah3004
@rosaliaimroatulmufidah3004 2 месяца назад
Hi, I want to ask how many ml is needed to wash the sample with 5% HCL?
@cigmmad
@cigmmad 2 месяца назад
Three Volumes. Some 150 ml each one.
@keerthishanmugam2218
@keerthishanmugam2218 7 месяцев назад
While adding KMnO4 to the graphite mixture, which color should be obtained? In my case, it is a dark green color. Is this ok or not?
@cigmmad
@cigmmad 7 месяцев назад
Yes, is the right color. Congrats!
@virajpasindu7806
@virajpasindu7806 5 месяцев назад
hi,, nice video in several articles i found that in modified hummers method we can add a 9:1 ratio of H2SO4 and H3PO4 mixture to the graphite. is this method a correct one with high purity and higher yield?
@cigmmad
@cigmmad 5 месяцев назад
Hi, the one you mention Is calles Marcano Method. We havent tried it to avoid using H3PO4 (very corrosive), but they are reports for good quality GO. Our method leds to good repeteability, good oxidation degree, very good dispersability in water, high exfoliation degree.
@nawelat418
@nawelat418 5 месяцев назад
Plz i did the synthesis based on modified hummers using graphite, H2SO4 and KMnO4 the solution became black at the end and after centrifugation I filtered the solution and i got something like powder and it's black before even i let it in the oven. where is the mistake ?
@cigmmad
@cigmmad 5 месяцев назад
Fast addition or KMnO4 during oxidation or if H2O2 and water at ehe end may reduce GO and turn black the suspension
@ridarida3154
@ridarida3154 3 месяца назад
Can you tell about DI water addition after 30 mint stirring at 35 °C. We should add is slowly and after cooling of mixture ?
@ridarida3154
@ridarida3154 3 месяца назад
As someone commented that it got fumes out in laboratory.
@cigmmad
@cigmmad 3 месяца назад
Because if you add it fast the reaction Will be fast and GO will became reduced
@ridarida3154
@ridarida3154 3 месяца назад
@@cigmmad we should add it in when flask in ice bath or in room temperature water (35°c )?
@nabaaanoor_
@nabaaanoor_ 11 месяцев назад
Can we use hot water bath temperature maintained at 98 ° C instead of antifreeze liquid or oil bath??
@cigmmad
@cigmmad 11 месяцев назад
Yes but it will be hard to avoid boiling and evaporation. You Will have to be adding extra water
@nabaaanoor_
@nabaaanoor_ 11 месяцев назад
Hi there, Before adding KMnO4 how many minutes should we stirr sulphuric acid with sodium nitrate and graphite powder?
@cigmmad
@cigmmad 11 месяцев назад
Enough to do an homogenous mixture. Nevertheless, this time shall influence the final amount of carboxyl groups, so if You have time You could try diferent times at this stage before KmNO4 addition
@nabaaanoor_
@nabaaanoor_ 11 месяцев назад
@@cigmmad alright, thanks!
@ridarida3154
@ridarida3154 3 месяца назад
Plz reply i want to know time bcz lots of ppl around me said it take 3-5 days to prepare Go. Is it true?
@cigmmad
@cigmmad 3 месяца назад
It takes a couple of days, synthesis, washing, drying
@priyankas4914
@priyankas4914 10 месяцев назад
Which oven is used for drying process? Microwave oven or hot oven? Is this possible to dry in 4 or 6hours using this oven?
@cigmmad
@cigmmad 10 месяцев назад
Hello. We use a "toaster" oven because we can control the temperature around 50oC si GO do not decompose, that is why it is si slow. In a microwave You have to test if temperature do not rise 50 oC. Of course is better a laboratory convection oven.
@priyankas4914
@priyankas4914 8 месяцев назад
Ok. thank you sir. What is the purpose of using NaNO3 in the initial chemical reaction? Is this possible to done this experiment without using sodium nitrate?
@cigmmad
@cigmmad 8 месяцев назад
Hello @@priyankas4914 well, there are several routes for GO synthesis. For example, there is one based on sulfuric and fosforic acid which not employ NaNO3, this is call the Marcano process. The purpose of NaNO3 is to separate the graphite layers and allow access to KMnO4 to oxidize the double bonds.
@rosellenunez6363
@rosellenunez6363 4 месяца назад
May I ask what's your % yield for this? thank you!
@cigmmad
@cigmmad 4 месяца назад
Hi, we got about 2 g of GO for each batch. It could be more but our centrifugation machine has only 4000 rpm so the lighter fractions (less sheet, more exfoliated GO) are lost.
@AnkurArunBhansali
@AnkurArunBhansali 11 месяцев назад
what is the antifreeze solution? and why is it added?
@cigmmad
@cigmmad 11 месяцев назад
The solution is a commercial antifreeze for cars, it is used to reach 98ºC without evaporation, thus we recommend the antifreeze with the highest possible boiling point. However, because of the generated fumes, it has to be done in fumehood to avoid health issues. Another option is to use a sand or an oil bath to safely reach 98ºC, it is question which one is easier to control; for oil is usually very dirty. I hope it is useful, let us know if you do the experiment and how it works for you.
@wedadali9359
@wedadali9359 6 месяцев назад
after 30 min, you added DI water to solution? when i did that the reaction was excited and the ash get out from flask to all lab
@cigmmad
@cigmmad 6 месяцев назад
Hi. No, we don't add water at that moment (30 min) but after the periods at 5 oC and 30 oC, the water is added and temperature is risen to 98oC. You added water to a highly reactive H2SO4 and KMnO4 mixture, that is why You get the violent reaction.
@wedadali9359
@wedadali9359 6 месяцев назад
ok thank you @@cigmmad
@wedadali9359
@wedadali9359 6 месяцев назад
and please is there any achieved method to get reduced graphene oxide
@cigmmad
@cigmmad 6 месяцев назад
@@wedadali9359yes, there are several and they depend on the level of reduction you want to achieve. For example you can use green reduction agents such as ascorbic acid, glucose, antioxidant additives (we can discuss options), or use hydrazine or NaBH4 if you have a lab with good safety as they are toxic or reactive.
@wedadali9359
@wedadali9359 6 месяцев назад
ok. actually I did that by NaBH4 , but the structure was not good , I mean I didn't get single layer. I have also question please, I want to know about temp. why should control it less than 10C,and then with rGO should increase it. Thank you
@28_fransiskusjulioalfonsos8
@28_fransiskusjulioalfonsos8 9 месяцев назад
Hi, thanks for the good videos. May i know, why you wash with HCl 5% solution? i mean i already make GO until the centrifuge steps. But my GO solution at 3 (pH), is with HCl solution can increase the pH of my GO solution? Or it will decrease the pH of my GO solution? Need the answer a.s.a.p if u don't mind hehe :)
@cigmmad
@cigmmad 9 месяцев назад
It is because You need to remove Mn ions and thereafter You rinse with DI water to remove Cl ions
@28_fransiskusjulioalfonsos8
@28_fransiskusjulioalfonsos8 9 месяцев назад
@@cigmmad thanks for the answer but i'm already used DI water and centrifuge before i use HCl solution. Is it ok? Let me know what matters if it is reversed🙏
@cigmmad
@cigmmad 9 месяцев назад
@@28_fransiskusjulioalfonsos8 well, with DI You won't be able yo remove most of Mn ions. If You want to try it and later compare with HCl rinsing and do some.elemental analysis to see ir only water removes Mn let me know.
@28_fransiskusjulioalfonsos8
@28_fransiskusjulioalfonsos8 9 месяцев назад
@@cigmmad thanks mate, i will do that later. hope u have a great day!
@cigmmad
@cigmmad 9 месяцев назад
@@28_fransiskusjulioalfonsos8 good luck!
@TyNguyen-yh4fe
@TyNguyen-yh4fe Год назад
what concentration of H2SO4 you use??
@cigmmad
@cigmmad Год назад
It is concentrated H2SO4, directly from the bottle, reactive or ACS grade.
@cigmmad
@cigmmad Год назад
lets us know if you get GO with this video!
@TyNguyen-yh4fe
@TyNguyen-yh4fe Год назад
@@cigmmad how can i contact you, i have a few question
@cigmmad
@cigmmad Год назад
@@TyNguyen-yh4fe send your email .ID, I willl contact you
@nabaaanoor_
@nabaaanoor_ 11 месяцев назад
Please mention volume of deionized water you have used in centrifugation process.
@cigmmad
@cigmmad 11 месяцев назад
We said "three volumes" because if the final volumen of the GO solution is, lets Say, 200 ml, we pour it in 15 mL centrufugue tubes and wash it three times
@nabaaanoor_
@nabaaanoor_ 11 месяцев назад
@@cigmmad ok got it
@cigmmad
@cigmmad 11 месяцев назад
We use three volumes considering the final volumen of the GO solution. We use 15 mL centrifugation tubes to pour Go
@cigmmad
@cigmmad 11 месяцев назад
@@nabaaanoor_ i hope it is useful and you can share your experience with us
@ridarida3154
@ridarida3154 3 месяца назад
How much time ( days ) taken by your experiment ?
@cigmmad
@cigmmad 3 месяца назад
Two days, synthesis one day, washing and drying second day.
@ridarida3154
@ridarida3154 3 месяца назад
@@cigmmad can you tell me it is a hummer method or modified one as research paper ( you have mentioned ) used the " term variation of hummer method" ? But not modified clearly
@cigmmad
@cigmmad 3 месяца назад
@@ridarida3154 we said "variation" because the reactants addition, how the H2O2-H2O mixture is added, how the material is washed are modifications of the Hummers report. You can check our paper here: 10.1016/j.matchemphys.2015.01.005
@ridarida3154
@ridarida3154 3 месяца назад
@@cigmmad ok thank you ✨stay blessed
@benedictekyamba
@benedictekyamba 8 месяцев назад
À la place de l'eau peut-on utilisé de l'éthanol ?
@cigmmad
@cigmmad 8 месяцев назад
No, on ne peut-pas parce-que l'ethanol i reaction fortement avec le acid sulphurique.
@benedictekyamba
@benedictekyamba 7 месяцев назад
Quand peut on utilisé l'éthanol
@cigmmad
@cigmmad 7 месяцев назад
on peut l'utilise apres le netoyage avec HCl 0.5 et apres H2O pour dehydrater le graphene oxide avant le mise au fourne, mais on peut avoir un peu de reduction de oxygene groups @@benedictekyamba
@cigmmad
@cigmmad 5 месяцев назад
Sure, send the steps.
@benedictekyamba
@benedictekyamba 7 месяцев назад
Quelle est la vitesse de rotation utilisée
@cigmmad
@cigmmad 7 месяцев назад
la machine a rotation n'a pas de scale de vitesse, mais on fixe la vitesse tel que un vortex aparait et tout se melange bien.(pardon pour mon Francais)
@harlenewatson45
@harlenewatson45 11 месяцев назад
What is graphene oxide used for?
@cigmmad
@cigmmad 11 месяцев назад
Applications range from energy storage, waste water treatment, water desalination, hydrogen generation, coatings for protection or electromagnetic management, drug delivery, sensors, composites and additives for plastics, between many more.
@user-mj2mh6hk8n
@user-mj2mh6hk8n 6 месяцев назад
Friend, I followed all the steps according to the article but the solution did not turn yellow or brown when adding the DI water together with the hydrogen peroxide
@cigmmad
@cigmmad 6 месяцев назад
I suppose your Solution Is black, yes? It happens when the KMnO4 is added very fast or if H2O AND H2O2 Is added suddenly. The color shall be greenish-yellowish, not net Green or Yellow
@user-mj2mh6hk8n
@user-mj2mh6hk8n 6 месяцев назад
I really made these mistakes, thank you, I will repeat the synthesis@@cigmmad
@cigmmad
@cigmmad 6 месяцев назад
@@user-mj2mh6hk8n ok, let me know if it worked!
@rosellenunez6363
@rosellenunez6363 Месяц назад
​@@cigmmadmine is too yellow, what do you think is my mistake?
@cigmmad
@cigmmad Месяц назад
@@rosellenunez6363 does It have sedimented material? Otherwise It could be fine. After rinsing and drying what color It has?
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