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

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

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.
SN/T 2379-2009
ENTRY-EXIT INSPECTION AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE 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 0.20??m 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 100??L 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 100??L 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) ?? 0.25??m (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: 1??L;
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.

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