GB/T 42310-2023 in English
VALIDNanotechnology—Measurement for specific surface area of graphene powder—Static volumetric method by argon gas adsorption
- Issued on:2023-03-17
- Implemented on:2023-10-01
- File Format:PDF
- Delivery:Via email within 5 business days
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《GB/T 42310-2023纳米技术 石墨烯粉体比表面积的测定 氩气吸附静态容量法》由TC279（全国纳米技术标准化技术委员会）归口，主管部门为中国科学院。
Introduction
Analysis of the core content of the standard
Principle of the method
Argon was used as the adsorbate, and the adsorption isotherm was measured by the static volumetric method at a liquid argon temperature of 87.3K. Based on the BET theory, the specific surface area was calculated by the formula SBET=3.82Vm, where Vm is the saturated adsorption capacity of the monolayer.
Comparison of key technologies
| Parameters | Argon adsorption method | Traditional nitrogen adsorption method |
|---|---|---|
| Adsorbate characteristics | No quadrupole moment, inert monatomic molecules | Diatomic molecules with quadrupole moment |
| Applicable samples | Graphene powder containing polar groups | Non-polar materials |
| Test deviation | Relative error <2% | Can reach more than 10% (Appendix A data) |
| Molecular cross-sectional area | 0.142nm² | 0.162nm² |
Instrument and material requirements
- Physical adsorption instrument: Calibration required, dead volume error ≤0.1cm³
- Analytical balance: Accuracy 0.1mg, anti-static treatment required
- Gas purity: Argon ≥99.995%, liquid argon ≥99.999%
Key steps of the test
- Sampling control: The total surface area should be kept in the range of 10-120m² (Example in Appendix C)
- Degassing: The maximum degassing temperature is determined by thermogravimetric analysis (Appendix D), and the vacuum degree is ≤1Pa
- Pressure point selection:
- Sample without micropores: 0.05-0.3 relative pressure range
- Sample with micropores: Find the linear interval in the range of 0.001-0.3 (Appendix E)
Special sample processing
Graphene powder containing micropores
Three conditions must be met:
- BET constant C＞0
- Va(1-p/p0) increases continuously with p/p0
- The pressure point corresponding to Vm is included in the selected point range
For a typical example, see the step-by-step point selection method in Appendix E of the standard.
Technology Evolution Background
The traditional nitrogen adsorption method causes specific adsorption due to defects and functional groups on the graphene surface (verified in Appendix A). Since argon molecules have no quadrupole moment, the difference in adsorption heat on polar surfaces is significantly lower than that of nitrogen (data in Appendix B), which is more in line with the ideal physical adsorption model.
Implementation Suggestions
- Laboratory environment: temperature fluctuation <5°C, humidity <60%RH
- Parallel sample requirements: at least 2 parallel samples, the deviation should be <3%
- Data verification: correlation coefficient R²≥0.999, C value must be positive
- Report content: must include degassing conditions, BET linear range, uncertainty assessment (requirements in Chapter 9)
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