Degassing time and temperature is an important step before BET analysis. as it removes moisture content and clears the pores and surface of the material to get correct data. Also, you can find data for graphene oxide in the literature.
The Brunauer-Emmett-Teller (BET) analysis is a common method used to determine the surface area of materials, including graphene oxide derived from biomass. The degassing time and temperature are critical parameters in BET analysis because they can significantly influence the accuracy and reliability of the measurements. Here's how they affect the process:
Degassing Time:
Removal of adsorbed species: Before conducting BET analysis, the sample must be degassed to remove adsorbed species like water, CO2, and other gases. Longer degassing times ensure more complete removal of these adsorbates, which can lead to a more accurate measurement of the surface area.
Stability of the sample: However, excessively long degassing times can sometimes damage the material, particularly if it is sensitive to vacuum conditions. This is less of a concern for graphene oxide but could be relevant for more delicate materials.
Equilibrium state: Adequate degassing time is necessary for the sample to reach a stable equilibrium state where no further gas or vapor is released. This stability is crucial for accurate BET measurements.
Degassing Temperature:
Removal efficiency: Higher temperatures typically increase the rate at which adsorbed molecules are removed from the sample's surface. This is because increased temperature provides the adsorbed molecules with more energy to overcome their adsorption potential.
Thermal stability: However, the temperature must be carefully controlled to avoid altering the sample's structure. Graphene oxide, for example, can undergo changes if exposed to too high temperatures, potentially affecting its surface properties and hence the BET results.
Optimal conditions: The optimal degassing temperature for graphene oxide derived from biomass would depend on the specific type of biomass and preparation method. It typically ranges from 100°C to 200°C, but specific conditions should be determined based on experimental results and literature.
In BET analysis of graphene oxide from biomass, finding the right balance between degassing time and temperature is essential. Insufficient degassing can lead to an overestimation of the surface area due to residual adsorbates, while excessive degassing can cause sample degradation or unnecessary experimental delays. The ideal conditions must be determined experimentally and may vary based on the sample's origin and treatment history. It's often recommended to follow established protocols in the literature for similar materials and adjust based on preliminary results.
Hello Ipah, I agree with what Dr. Ganachari explained, so much is that as it is a material that has already been transformed into graphene oxide, this material will no longer behave like a common carbonaceous material, as materials such as biomass or even Even carbon that has not been activated or transformed into some other material, can be treated at temperatures above 100 °C, the ideal for these materials (graphene oxides or activated carbon) is temperatures of 150 to 180 °C for 8 to 12 hours another detail that you have to keep an wacthful on is which analysis gas will be adopted and its purity, as these parameters also influence the analysis, a quantity of material that is used for analysis ~ 150 mg is already a quantity enough for BET analysis, of course depending on the sample holder, the good thing about this characterization is that you don't "lose the sample"