GB/T 38592-2020 in English
VALIDDetermination of 4,4′-methylene-bis(2-chloroaniline)in textile dyeing and finishing auxiliaries
- Issued on:2020-03-31
- Implemented on:2021-02-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$127.00
《GB/T 38592-2020纺织染整助剂产品中4,4'-亚甲基双(2-氯苯胺)的测定》由TC134(全国染料标准化技术委员会)归口,TC134SC1(全国染料标准化技术委员会印染助剂分会)执行,主管部门为中国石油和化学工业联合会。
Introduction
Standard background and scope of application
This standard establishes a detection method for the potential carcinogen 4,4'-methylenebis(2-chloroaniline) (MOCA) in textile dyeing and finishing auxiliaries, which is applicable to the quality control of various auxiliary products. As the core content of GB/T 38592-2020, the method uses gas chromatography-triple quadrupole mass spectrometry to achieve a detection limit of 10 mg/kg.
Key technical principles
MOCA in the sample is extracted by ultrasonic toluene, and after treatment with anhydrous sodium sulfate and sodium oxide, the multiple reaction monitoring mode (MRM) of GC-MS/MS is used for qualitative and quantitative analysis. The characteristic ion pairs m/z 231→195 (quantitative) and m/z 266→195 (qualitative) ensured the detection specificity.
| Technical Parameters | Requirements of this Standard | Conventional HPLC Method |
|---|---|---|
| Detection Limit | 10 mg/kg | 50 mg/kg |
| Recovery | 80%-110% | 70%-120% |
| Precision | RSD≤10% | RSD≤15% |
Key Operation Steps
- Sample pretreatment: 0.2g sample was dissolved in 5mL water, 2g anhydrous sodium sulfate and sodium oxide were added, and 10mL toluene was ultrasonically extracted for 15min
- Centrifugal purification: 10000r/min centrifugation for 10min, 0.22μm filter membrane filtration
- Instrumental analysis: VF-5MS chromatographic column (30m×0.25mm×0.25μm), 60-280℃ programmed temperature, MRM mode detection
Implementation points
Standard solution preparation: 1000mg/L stock solution should be stored at 4℃ away from light, and the working solution should be prepared and used immediately. It is recommended to establish a 5-point standard curve of 0.1-20mg/L.
Quality control requirements: Each batch of samples should include blank controls and spike recovery experiments, and the recovery rate should be controlled within the range of 80%-110%.
Technology evolution analysis
Compared with the traditional HPLC method, this standard has three major advantages: 1) detection sensitivity is increased by 5 times; 2) matrix interference is eliminated through characteristic ion pairs; 3) analysis time is shortened to 14 minutes. The total ion current chromatogram and multiple reaction monitoring mass spectrum provided in Appendix A can be used as a reference for method validation.

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