SN/T 4765-2017 in English
VALIDFood contact materials—Polymers—Determination of hexachloro-1,3-butadiene—Gas chromatography-mass spectrometry
- Issued on:2017-05-12
- Implemented on:2017-12-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$117.00
Introduction
Technical Background of the Standard
This standard is formulated for hexachloro-1,3-butadiene (HCBD) that may migrate in polymer materials for food contact. This substance is listed as a potential carcinogen by the WHO. It was issued and implemented in 2017, filling the gap in my country's testing standards in this field.
Core principles of the method
| Technical aspects | Key parameters | Innovation points |
|---|---|---|
| Sample pretreatment | Liquid nitrogen freezing and crushing + ultrasonic dichloromethane extraction | Double extraction guarantees recovery rate ≥85% |
| GC-MS analysis | HP-5MS chromatographic column + SIM mode | Detection limit as low as 0.01mg/kg |
| Mass spectrometry qualitative analysis | m/z 225/227 characteristic ion ratio | ±20% deviation control |
Key operating points
Instrument parameter optimization
Programmed temperature (40℃→270℃) combined with 70eV ionization energy of EI source was used to ensure baseline separation of HCBD at 8-9min. Actual cases show that when the carrier gas flow rate deviates from 1.2mL/min±10%, the retention time drift can reach 0.5min.
Quality control requirements
- Blank test value should be ＜30% of the lower limit of determination of the method
- Correlation coefficient of standard curve R²≥0.995
- The spike recovery rate is controlled at 80-110%
Method validation data
| Material type | Repeatability RSD(%) | Reproducibility RSD(%) | Actual detection limit |
|---|---|---|---|
| PP plastic | 6.8 | 12.3 | 0.008mg/kg |
| Silicone rubber | 7.5 | 13.7 | 0.009mg/kg |
Implementation recommendations
- Laboratories should regularly verify the calibration of the mass axis of the mass spectrometer to ensure that the mass deviation between m/z 225 and 227 is less than 0.1amu
- For high-fat samples, it is recommended to add a Florisil column cleanup step
- When testing PE materials, the extraction time can be extended to 40min
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