GB 31604.27-2016_English: PDF (GB31604.27-2016)
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Food contact materials -- Determination of ethylene oxide and propylene oxide in plastics -- Gas chromatography
| Valid |
GB 31604.27-2016
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Standards related to: GB 31604.27-2016
| Standard ID | GB 31604.27-2016 (GB31604.27-2016) | | Description (Translated English) | Food contact materials -- Determination of ethylene oxide and propylene oxide in plastics -- Gas chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | X09 | | Word Count Estimation | 12,136 | | Date of Issue | 2016-10-19 | | Date of Implementation | 2017-04-19 | | Older Standard (superseded by this standard) | GB/T 23296.11-2009 | | Regulation (derived from) | State Health and Family Planning Commission Notice No.1516 of 2016 | GB 31604.27-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food contact
materials and products - Determination of ethylene
oxide and epoxy propane in plastics
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of People's
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 6
5 Analytical steps ... 6
6 Expression of the analytic result ... 9
7 Precision... 10
8 Others ... 10
9 Principle... 10
10 Reagents and materials... 10
11 Instruments and equipment ... 12
12 Analytical steps ... 12
13 Expression of the analytic result ... 15
14 Precision ... 15
15 Others ... 16
Appendix A Standard chromatogram of ethylene oxide and epoxy propane 17
National Food Safety Standard - Food contact materials
and products - Determination of ethylene oxide and
epoxy propane in plastics
1 Scope
This standard specifies the methods of determination of ethylene oxide and
epoxy propane in food contact materials and products.
This standard is applicable to the determination of ethylene oxide and epoxy
propane in plastic food contact materials and products.
The first method -
Headspace gas chromatography-mass spectrometry
2 Principle
After ethylene oxide or epoxy propane being extracted by N, N-dimethyl
acetamide (DMAC), introduce it in the sample by headspace injection.
Separate the ethylene oxide or epoxy propane from the internal standard
diethyl ether and other components in the chromatographic column. Detect
with spectrum detector, determine the quantity by internal standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method shall be analytical
pure. The water shall be the primary water specified in GB/T 6682.
3.1 Reagents
N, N-dimethyl acetamide (DMAC, C4H9NO, CAS. 127-19 -5). color spectrum
pure. The area of the impurity peak with the same retention time of ethylene
oxide or epoxy propane shall not exceed 1%.
3.2 Standard product
3.2.1 Ethylene oxide (C2H4O, CAS. 75-21-8). purity ≥99%, or a standard
2.0μg/mL, 4.0μg/mL; the concentrations of epoxy propane are respectively
0.05μg/mL, 0.1μg/mL, 0.2μg/mL, 0.5μg/mL, 1.0μg/mL, 2.0μg/mL. The
storage condition of the solution is the same as 3.3.1.
3.3.5 Diethyl ether internal standard reserve solution
Weigh 50 mg (precision to 0.0001 g) of diethyl ether, put into a 50mL
volumetric flask containing 5mL of DMAC. Meter with DMAC and obtain the
reserve solution with concentration of 1 mg/mL. The storage condition of the
solution is the same as 3.3.1.
3.3.6 Diethyl ether internal standard intermediate solution
Weigh 5mL of DMAC and put into a 10mL volumetric flask, then draw with
graduated pipette 2.5mL of the diethyl ether internal standard reserve solution
(3.3.5) and put into the volumetric flask. Meter with DMAC and obtain the
diethyl ether internal standard intermediate solution. The concentration is
250.0μg/mL. The storage condition of the solution is the same as 3.3.1.
4 Instruments and equipment
4.1 Gas chromatography-mass spectrometer. equipped with electron
bombardment ion source (EI) and headspace automatic sampler.
4.2 Micro-syringe. 10μL, 100μL, 1000μL;
4.3 Headspace bottle. 20mL, equipped with aluminum cap and butadiene
rubber or silicone rubber spacer. The spacer shall be coated with
polytetrafluoroethylene on the side contacting sample.
4.4 Analytical balance. sensitivity 0.0001g.
4.5 Mechanical oscillator.
5 Analytical steps
5.1 Sample treatment
The sample soluble in DMAC shall be weighed directly. The sample which is
not soluble in DMAC shall be crushed to a particle size smaller than 1mm×
1mm by cutting tools such as cryogenic grinder or scissors, and be weighed
as soon as possible. When cutting the sample, shall not make it heated and
soft.
5.2 Preparation of sample solution
e) Carrier gas. helium.
5.4.3 Mass spectrometry conditions
The mass spectrum conditions are as follows.
a) Mass spectrum interface temperature. 280°C;
b) Quadrupole rod temperature. 150°C;
c) Ionization mode. EI;
d) Ionization energy. 70 eV;
e) Determination method. select ion monitoring mode, monitor ion range.
m/z 15 ~ m/z 100. The qualitative ions of ethylene oxide are 15, 29, 43,
44, of which 44 is quantitative ion; the qualitative ions of epoxy propane
are 28, 31, 43, 58, of which 58 is quantitative ion; the qualitative ions of
diethyl ether are 31, 45, 59, 74, of which 74 is quantitative ion.
5.5 Making of standard curve
Draw with graduated pipette 5.0 mL of ethylene oxide and epoxy propane
mixed standard solution (3.3.4) to 6 headspace bottles respectively. Add
respectively with micro-syringe 10μL internal standard intermediate solution
of diethyl ether (3.3.6) and seal with cover as soon as possible. Under the
conditions provided in 5.4, put the above solutions respectively through
headspace gas chromatography-mass spectrometer to determine. Use the
concentrations of ethylene oxide (or epoxy propane) in the solution as
abscissa in unit of microgram per milliliter (μg/mL) and the peak area ratio of
ethylene oxide (or epoxy propane) to diethyl ether as ordinate to draw
standard curves respectively. See A.1 for standard chromatogram.
5.6 Determination of sample solution
Inject the sample solution and blank solution into the headspace gas
chromatography-mass spectrometer to determine the peak area ratio of
ethylene oxide (or epoxy propane) to diethyl ether. Obtain the concentration
of ethylene oxide (or epoxy propane) in sample solution from the standard
curve.
5.7 Qualitative
When determine the sample under the same experimental conditions, if the
deviation of the chromatographic peak retention time of the substance to be
determined in the sample solution is within ±2.5% of the chromatographic
peak retention time of the standard substance; and all the selected ions
10.2.1 Ethylene oxide (C2H4O, CAS. 75-21-8). purity ≥99%, or a standard
substance certified by the State and granted the standard substance
certificate.
10.2.2 Epoxy propane (C3H6O, CAS.200-879-2). purity ≥99%, or a standard
substance certified by the State and granted the standard substance
certificate.
10.2.3 Diethyl ether (C4H10O, CAS. 60-29-7). purity ≥99.5%, or a standard
substance certified by the State and granted the standard substance
certificate. The area of the impurity peak with the same retention time of
ethylene oxide or epoxy propane shall not exceed 1%.
10.3 Standard solution preparation
10.3.1 Ethylene oxide standard reserve solution
Weigh 50 mg (precision to 0.0001 g) of ethylene oxide, dissolve with DMAC,
meter the volume to 50 mL, obtain the reserve solution with concentration of
1mg/mL. Store the solution at 4°C sealed and keep away from light. The
validity period is 2 months.
10.3.2 Epoxy propane standard reserve solution
Weigh 50 mg (precision to 0.0001 g) of epoxy propane, dissolve with DMAC,
meter the volume to 50 mL, obtain the reserve solution with concentration of
1mg/mL. Store the solution at 4°C sealed and keep away from light. The
validity period is 2 months.
10.3.3 Mixed standard intermediate solution of ethylene oxide and
epoxy propane
Draw 5.0mL of DMAC and put into 6 10mL volumetric flasks respectively.
Draw with micro-syringe respectively 0μL, 40μL, 100μL, 200μL, 300μL,
400μL of the ethylene oxide standard reserve solution (10.3.1) and put into
the above-mentioned 6 volumetric flasks respectively. Draw with
micro-syringe 0μL, 40μL, 100μL, 200μL, 300μL, 400μL of the epoxy propane
standard reserve solution (10.3.2) and put into the above-mentioned 6
volumetric flasks respectively. Meter with DMAC to the scale. Thus, obtain the
mixed standard intermediate solution of ethylene oxide and epoxy propane.
The concentrations of ethylene oxide are respectively 0μg/mL, 4μg/mL,
10μg/mL, 20μg/mL, 30μg/mL, 40μg/mL; the concentrations of epoxy propane
are respectively 0μg/mL, 4μg/mL, 10μg/mL, 20μg/mL, 30μg/mL, 40μg/mL.
The storage condition of the solution is the same as 10.3.1.
10.3.4 Diethyl ether internal standard reserve solution
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