GB/T 39114-2020 in English
VALIDNanotechnologies—Characterization of single-wall carbon nanotubes using ultraviolet-visible-near infrared (UV-Vis-NIR) absorption spectroscopy
- Issued on:2020-10-11
- Implemented on:2021-05-01
- File Format:PDF
- Delivery:Via email within 5 business days
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《GB/T 39114-2020纳米技术 单壁碳纳米管的紫外/可见/近红外吸收光谱表征方法》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
Technical background and evolution of standards
This standard is equivalent to the ISO/TS10868:2017 international technical specification, marking that my country's nanomaterial characterization technology is in line with international standards. As a non-destructive characterization method, the development of UV/Vis/NIR absorption spectroscopy has gone through three stages:
| Development stage | Technical characteristics | Breakthrough progress |
|---|---|---|
| Early stage (1998-2005) | Qualitative identification of characteristic peaks | Discovery of S11/S22/M11 transition peaks |
| Mid-term (2006-2012) | Semi-quantitative analysis | Establishment of diameter-peak position relationship model |
| Current stage (2013-) | Standardized measurement | Establish a purity index calculation method |
Core parameter measurement principle
Diameter determination method
Diameter calculation formula derived from tight binding theory:
d = 1.7/Eg(S22) (nm/eV)
d = 2.6/Eg(M11) (nm/eV)
Note in actual application:
- The error is minimum when the diameter measurement range is 1-2nm
- For samples above 1.4nm, the solid thin film method is recommended
- The bundle effect will increase the peak width by 10-15%
Purity index calculation
The purity index Pi reflects the mass fraction of SWCNTs in the total carbon content:
Calculation step case: A sample in the range of 7000-17000cm-1:
- Total integrated area AAt=662
- S22 characteristic peak area AA(S22)=40
- Pi=40/662≈0.060
Special attention should be paid:
- DMF solvent must be strictly dehydrated
- Baseline selection should avoid interference from the 8000cm-1 water peak
- Different batches of samples should maintain the same diameter distribution
Key Experimental Operation Specifications
Key Points of Sample Preparation
| Test Objective | Dispersion System | Key Parameters |
|---|---|---|
| Diameter/Metallicity Ratio | D2O+Surfactant | Centrifugal Force ≥120000×g |
| Purity Index | DMF Dispersion | Final Concentration 0.01mg/mL |
| Large Diameter Sample | CMC Film | Drying Temperature ≤50℃ |
Implementation suggestions and precautions
Measurement uncertainty control
Main error sources and countermeasures:
- Tube bundle effect: Ultracentrifugation time extended to 5h
- Solvent interference: D2O purity ≥99.9%
- Instrument calibration: Warm-up time ≥1h
- Temperature effect: Ice bath temperature control is required during ultrasound
Data reporting requirements
A complete report must include:
- Specific transition peak type used (S11/S22/M11)
- Ultracentrifugation parameters (speed/time/rotor type)
- Spectral integration energy range
- Description of baseline determination method
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