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polyfluorinated compounds heat-resisting material introduction technical background method validation data standard validation shows internal standard liquid chromatography-mass spectrometry/mass spectrometry μg/kg 1 2 3 4-13c4 perfluorooctanoic acid gas chromatography-mass spectrometry/mass spectrometry finish content second-generation diazo strain-type linear displacement transducer
SN/T 5352-2021 in English

SN/T 5352-2021 in English

VALID

Determination of perfluorinated and polyfluorinated compounds in paper heat-resisting material

  • Issued on:2021-11-22
  • Implemented on:2022-06-01
  • File Format:PDF
  • Delivery:Via email within 5 business days
Price(USD): $570.00
$553.00
Standard No: SN/T 5352-2021
Document status: VALID
Title in English: Determination of perfluorinated and polyfluorinated compounds in paper heat-resisting material
Title in Chinese: 纸制耐热材料中全氟和多氟化合物的测定
Language: English
File Format: Electronic (PDF)
Delivery: Via email within 5 business days
Issued on: 2021-11-22
Implemented on: 2022-06-01
Professional Classification: SN-Import&Export Inspection
Related Keywords: polyfluorinated compounds
heat-resisting material introduction technical background
method validation data standard validation shows
internal standard liquid chromatography-mass spectrometry/mass spectrometry
μg/kg 1
2
3
4-13c4 perfluorooctanoic acid gas chromatography-mass spectrometry/mass spectrometry
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Introduction

Technical Background of the Standard

With the widespread application of per- and polyfluorinated compounds (PFCs) in the industrial field, their environmental persistence and bioaccumulation have attracted global attention. This standard was formulated under the leadership of the General Administration of Customs and established a dual-platform detection scheme for 36 PFCs in paper heat-resistant materials, filling the gap in my country's detection methods in this field.


Core elements of the method

Detection platform Number of targets Limit of quantification Selection of internal standard
Liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) 27 species 5 μg/kg 1,2,3,4-13C4 perfluorooctanoic acid
Gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS) 9 species 10 μg/kg Methyl heptadecanoate-d33

Key operating points

Sample pretreatment process

  1. Extraction: 2-4g sample was extracted by ultrasonic extraction with methanol (60℃, 60min)
  2. Concentration: Rotary evaporation to 2mL under 250mbar
  3. Purification: 0.2μm organic phase filter membrane filtration

Instrument parameter optimization

LC-MS/MS adopted electrospray negative ionization mode, gradient elution program: 0-3min 10%B → 18min 100%B (mobile phase A: water, B: methanol)
GC-MS/MS uses a DB-5MS column with a programmed temperature of 75℃(3min)→300℃(5min)


Method validation data

Standard validation shows:
• Spike recovery: 70%-120%
• Repeatability RSD<15%
• Reproducibility RSD<20%
At a typical compound PFOS spike level of 20μg/kg, the reproducibility is 3.79% and the reproducibility is 19.6%


Implementation recommendations

  • The laboratory needs to establish a mass calibration procedure for the triple quadrupole mass spectrometer
  • It is recommended that each batch of samples be accompanied by process blanks and matrix spikes
  • Note that substances such as perfluorooctane sulfonic acid (PFOS) have isomer interference

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