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textile dyeing finishing auxiliaries auxiliaries introduction standard background standard conventional hplc method detection limit mrm mode detection implementation points standard solution preparation relevant safety standards interface data transcranial doppler hematology analyzers
GB/T 38592-2020 in English

GB/T 38592-2020 in English

VALID

Determination 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
Price(USD): $130.00
$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

  1. 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
  2. Centrifugal purification: 10000r/min centrifugation for 10min, 0.22μm filter membrane filtration
  3. 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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