SN/T 2379-2009 English PDF (SNT2379-2009)

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SN/T 2379-2009: Determination of bisphenol A in polycarbonate resin and its products. Gas chromatography-mass spectrography
SN/T 2379-2009
ENTRY-EXIT INSPECTION AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA
Determination of Bisphenol A in Polycarbonate Resin
and Its Products – Gas Chromatography-Mass
Spectrometry
ISSUED ON: SEPTEMBER 02, 2009
IMPLEMENTED ON: MARCH 16, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method Summary ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Preparation of the Sample ... 5
6 Analytical Procedures ... 5
7 Calculation of Results ... 7
8 Lower Limit of Detection ... 8
9 Precision ... 8
Appendix A (Informative) Gas Chromatography – Mass Spectrometry Diagram
of Pentafluoropropionated Bisphenol A Derivative ... 9
Determination of Bisphenol A in Polycarbonate Resin
and Its Products – Gas Chromatography-Mass
Spectrometry
1 Scope
This Standard specifies determination of bisphenol A in polycarbonate resin and its
products by gas chromatography-mass spectrometry.
This Standard is applicable to the determination of bisphenol A in polycarbonate resin
and its products.
2 Method Summary
Acetone was used as the extraction solvent for the specimen. After ultrasonic
extraction, derivatization was carried out by pentafluoropropionic anhydride. The
solution was blown dry by nitrogen. Use n-hexane to make constant volume; and
analyzed by gas chromatography-mass spectrometry.
3 Reagents and Materials
3.1 Acetone: chromatographically pure.
3.2 n-hexane: chromatographically pure.
3.3 Pentafluoropropionic anhydride: purity ≥98%.
3.4 Bisphenol A standard product: CAS: 80-05-7, purity ≥99%.
3.5 Bisphenol A standard stock solution: accurately weigh 10mg of bisphenol A
standard (3.4); place it in a 100mL volumetric flask; dilute to the mark by acetone (3.1);
and mix well. The concentration of this solution is 100g/L.
3.6 Preparation of standard working solution: respectively pipette appropriate volume
of bisphenol A standard stock solution (3.5); dilute by acetone (3.1) to prepare standard
working solution with required concentration.
at 4000 r/min for 15 min in a centrifuge (4.7). Absorb the supernatant by a syringe (4.8);
pass the injecting solution through a 0.20µm organic filter membrane (4.9); and collect
the filtrate in a brown bottle. Pipette 1mL of the filtrate to a graduated centrifuge tube
accurately; add 100µL of derivatization reagent pentafluoropropionic anhydride (3.3);
place in a vortex mixer (4.10) and vortex to mix; derivatize in a constant temperature
water bath (4.11) at 60°C for 30min. After that, place it in a nitrogen blower (4.12) and
slowly blow it to near dryness. Add 1mL of n-hexane (3.2); vortex to mix; and transfer
the solution to the sample injecting bottle for gas chromatography-mass spectrometry
detection.
6.3 Preparation of standard working solution
Accurately transfer a certain volume of standard solution with the appropriate
concentration to the graduated centrifuge tube (4.6); add 100µL of the derivatization
reagent pentafluoropropionic anhydride (3.3); and follow the 6.2 derivatization
procedures below.
6.4 Gas chromatography – mass spectrometry conditions
6.4.1 Chromatographic column: 30m × 0.25mm (inner diameter) × 0.25µm (film
thickness); HP-5MS quartz capillary column or equivalent.
6.4.2 Chromatographic column temperature: initial temperature is 70°C, maintain for
1min; then raise the temperature to 210°C at 30°C/min; and then raise the temperature
to 260°C at 10°C/min, and maintain for 2min.
6.4.3 Inlet temperature: 260°C;
6.4.4 Mass spectrometer interface temperature: 280°C;
6.4.5 Carrier gas: helium, purity ≥99.99%; flowrate of 1.0mL/min;
6.4.6 Sample injecting method: split-less injection; open the valve after 1.0min;
6.4.7 Sample injecting quantity: 1µL;
6.4.8 Electric ionization method: EI;
6.4.9 Electric ionization energy: 70eV;
6.4.10 Determination method: selective ion monitoring method;
6.4.11 Select monitoring ion (m/z): 265, 505, 520;
6.4.12 Solvent delay time: 5min.
6.5 Gas chromatography – mass spectrometry determination
M – specimen mass, in g.
8 Lower Limit of Detection
This method’s lower limit of the detection is 0.05 mg/kg.
9 Precision
Determine the reliability of the results (95% confidence level) as follows:
9.1 Repeatability
In the same laboratory, the same person uses the same equipment, the same test
method, and the absolute difference between the two parallel determination results of
the same test object within the day is no greater than 10% of the arithmetic mean of
the two measured values.
9.2 Reproducibility
In different laboratories, the same person uses the same equipment and the same test
method. The absolute difference between two parallel measurements of the same
object is no greater than 15% of the arithmetic mean of the two measured values.