SN/T 5257-2019 in English
VALIDDetermination of Di- -n- octyltin-bis (2-ethylhexyl thiogiy-clloate)in plastics and plastics articles- Gas chromatography- mass spectrometry
- Issued on:2019-12-27
- Implemented on:2020-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$127.00
Introduction
Technical background and scope of application of the standard
This standard (SN/T 5257-2019) was proposed by the General Administration of Customs and formulated to meet the detection requirements of organic tin compounds in plastic products - di-n-octyltin 2-ethylhexyl thioglycolate (DOTE). This method is applicable to plastic materials soluble in tetrahydrofuran, with a minimum determination limit of 2.0 mg/kg, providing a technical basis for the safety supervision of imported and exported goods.
Core method principle
| Steps | Key technologies | Parameter requirements |
|---|---|---|
| Sample pretreatment | Tetrahydrofuran dissolution-methanol precipitation method | Ultrasonic extraction ≥30min, centrifugation>5000r/min |
| Derivatization reaction | Sodium tetraethylborate derivatization | pH=4.0±0.1, reaction 15min |
| Instrumental analysis | GC-MS coupling | DB-5MS chromatographic column, EI ion source |
Analysis of key operation points
Sample preparation specifications
The sample needs to be cut into pieces of 1mm×1mm and accurately weighed to 0.5g. Note:
- The volume ratio of tetrahydrofuran to methanol is 1:2
- After precipitation, three methanol washes are required to ensure the recovery rate
- The rotary evaporation temperature is controlled below 40°C
Instrument parameter optimization
The standard recommendation is to use a DB-5MS capillary column (30m×250μm×0.10μm), and the programmed temperature setting is:
- Initially maintain 60°C for 1min
- Raise to 220°C at 20°C/min (4min)
- Then raise to 280°C at 20°C/min (5min)
Method validation data
Collaborative validation by 6 laboratories showed:
- Linear range: 10-200μg/mL (R²>0.995)
- Repeatability limit: 0.005m+1.935
- Reproducibility limit: 0.061m+0.135
Implementation suggestions
Interference elimination plan
When detecting 2-ethylhexyl thioglycolate (by-product):
- Ethyl acetate extraction should be performed simultaneously
- Monitor characteristic ions 71/43/112
- Retention time deviation should be <0.2min
Quality control requirements
Each batch of testing should include:
- Method blank control
- Spike recovery experiment (spike amount 10-50μg/mL)
- Parallel sample determination (RSD≤15%)
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