GB/T 38397-2019 in English
VALIDCoal tar—Determination of component content—Gas chromatography-mass spectrometry and thermogravimetry
- Issued on:2019-12-31
- Implemented on:2020-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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《GB/T 38397-2019煤焦油 组分含量的测定 气相色谱-质谱联用和热重分析法》由TC469（全国煤化工标准化技术委员会）归口，TC469SC3（全国煤化工标准化技术委员会炼焦化学分会）执行，主管部门为国家标准化管理委员会。
Introduction
Technical background of the standard
This standard aims at the precise needs of component analysis in the process of coal tar processing and utilization, and combines the development of modern analytical technology to establish a collaborative detection system of gas chromatography-mass spectrometry (GC-MS) and thermogravimetric analysis (TGA). Compared with the traditional method, the 2019 version of the standard adds a mass compensation mechanism of thermogravimetric analyzer to solve the problem of detection deviation caused by incomplete vaporization of high-temperature components.
Comparison of core methods
| Technical parameters | GC-MS | TGA | Synergistic advantages |
|---|---|---|---|
| Detection object | Qualitative and quantitative analysis of vaporized components | Mass change monitoring | Full characterization of vaporized/residual components |
| Temperature control | 300℃ final temperature | Synchronous heating program | Data temporal and spatial consistency |
| Accuracy requirements | 0.1u mass resolution | 0.01mg resolution | Cross-validation reliability |
Key operating points
Sample preparation specifications
Dehydration treatment must strictly follow GB/T260-2016, medium and low temperature coal tar is dissolved with dichloromethane, and high temperature coal tar is dissolved with tetrahydrofuran. The ultrasonic dissolution time is controlled at 2±0.5 minutes, and a 0.45μm organic syringe filter must be used in the filtration process.
Instrument parameter optimization
- GC-MS carrier gas flow rate: 1.0mL/min (He gas purity ≥99.9995%)
- TGA protection gas flow rate: 20mL/min (N₂ purity ≥99.99%)
- Four-stage heating program: 10℃/min→3℃/min gradient change
Data processing model
Component content calculation formula: W=Q×M/100, where:
- Q: Final thermal weight loss rate measured by TGA
- M: GC-MS peak area normalization result
Repeatability requirements for typical components: 1,2-dimethylnaphthalene ≤ 0.742%, phenanthrene ≤ 0.697%, data rounding shall be performed according to GB/T8170.
Safety implementation recommendations
- Radioactive protection: Wear a dose meter when operating gas chromatograph-mass spectrometer
- Poison control: Dichloromethane dissolution should be completed in a fume hood
- Temperature warning: Double isolation device is set in the 300℃ high temperature area
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