SN/T 5229-2019 in English
VALIDLeather- Screening of heavy metals ( Pb、Cd. Hg、Cr)-Energy dispersive X-ray fluorescence spectrometric method
- Issued on:2019-12-27
- Implemented on:2020-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$117.00
Introduction
Technical Background of the Standard
With the improvement of safety requirements for children's toys, the detection of isothiazolinone preservatives (MI/CMI/BIT) has become a focus of international attention. This standard uses liquid chromatography-mass spectrometry to establish a high-sensitivity detection method, which makes up for the limitations of traditional HPLC methods in complex matrices.
Key Detection Parameters
| Component | Detection Limit (mg/kg) | Quantitative Ion Pair (m/z) | Chromatographic Retention Time (min) |
|---|---|---|---|
| MI | 0.075 | 116.0→71.4 | 2.18 |
| CMI | 0.075 | 149.9→87.2 | 3.38 |
| BIT | 0.030 | 152.0→109.1 | 4.45 |
Key points for sample pretreatment
Typical case: An exported plastic toy was found to have excessive CMI. After review, it was found that the ultrasonic extraction time was insufficient. The 20-minute ultrasonic extraction required by the standard was used in conjunction with polypropylene test tubes to effectively avoid adsorption losses.
- Aqueous liquid: directly dilute and then filter
- Stickers: need to be cut into <3mm pieces
- Clay/leather: representative sampling must be ensured
LC-MS condition optimization
Use a C18 column (2.1×150mm) with methanol-0.1% formic acid water (45:55) isocratic elution, in ESI+ mode:
- Capillary voltage 4000V
- Ion source temperature 350℃
- SRM mode acquisition for 8 minutes
Implementation suggestions
Laboratories should pay attention to:
- Regularly calibrate the mass axis of the mass spectrometer
- Using isotope internal standards can improve quantitative accuracy
- Toys made of different materials need to verify recovery rates separately
After the implementation of this standard, toy companies should establish a raw material preservative screening system, paying special attention to high-risk materials such as water-based coatings and adhesives.
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