GB 31604.17-2016National food safety standard - Food contact materials and articles - Determination of the content and migration of acrylonitrile (English PDF)
食品安全国家标准 食品接触材料及制品 丙烯腈的测定和迁移量的测定
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Issued by
National Health and Family Planning Commission of the PRC
Level / Type
National · Mandatory
Issue date
October 19, 2016
Implementation date
April 19, 2017
Scope
GB 31604.17-2016 is the English-translated version of 食品安全国家标准 食品接触材料及制品 丙烯腈的测定和迁移量的测定.
GB 31604.17-2016 — This standard specifies the method for determination of the content and migration of acrylonitrile in food contact materials and articles. This standard applies to the determination of the content and migration of acrylonitrile in food contact materials and articles. Determination of acrylonitrile
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Document preview — GB 31604.17-2016
National Standard of the People's Republic of China
Issued by: National Health and Family Planning Commission of the PRC
Contents
- Foreword...3
- 1 Scope...4
- 2 Principle...4
- 3 Reagents and materials...4
- 4 Instruments and equipment...5
- 5 Analytical procedures...5
- 6 Expression of analysis results...7
- 7 Precision...7
- 8 Others...8
- 9 Principle...8
- 10 Reagents and materials...8
- 11 Instruments and equipment...9
- 12 Analytical procedures...9
- 13 Expression of analysis results...11
- 14 Precision...11
- 15 Others...11
- Appendix A Acrylonitrile gas chromatogram...12
Foreword
This standard replaces GB/T 5009.152-2003 "Determination of residual
acrylonitrile monomer in styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their products used for foods pack"
and GB/T 23296.8-2009 "Food contact materials - Polymer - Determination of
acrylonitrile in food simulants - Gas chromatography" and SN/T 2197-2008
"Food contact materials - Polymer materials - Determination of acrylonitrile in
food and food simulants - Gas chromatography".
As compared with GB/T 5009.152-2003, the main changes of this standard are
as follows.
- CHANGE the standard name into "National food safety standard - Food
contact materials and articles - Determination of the content and migration
of acrylonitrile";
- DELETE the gas chromatography-hydrogen flame detector method,
RETAIN the gas chromatography-nitrogen phosphorus detector method;
- ADD the determination of the migration of acrylonitrile in food contact
materials and articles.
National food safety standard –
Food contact materials and articles –
Determination of the content and migration of acrylonitrile
1 Scope
This standard specifies the method for determination of the content and
migration of acrylonitrile in food contact materials and articles.
This standard applies to the determination of the content and migration of
acrylonitrile in food contact materials and articles.
Determination of acrylonitrile
2 Principle
The food contact materials and articles are dissolved or dispersed in a
headspace flask via N,N-dimethylformamide, heated to allow the components
to be tested to reach a gas-liquid equilibrium, then the top air is quantitatively
sucked for gas chromatographic determination. The retention time is based for
qualitative determination, the propionitrile is used as internal standard, the
internal standard method is used for quantitative determination.
3 Reagents and materials
The water used in this method is grade I water specified in GB/T 6682.
Containers and transfer apparatus used in the test shall avoid the use of plastic
materials.
3.1 Reagents
N,N-dimethylformamide (DMF). analytically pure, no interference peaks at the
retention times of acrylonitrile and propionitrile.
3.2 Standard substance
3.2.1 Acrylonitrile (C3H3N, CAS No.. 107-13-1). 1000 µg/mL, or a standard
substance that is certified by the state and granted a standard substance
certificate.
3.3 Standard solution preparation
4 Instruments and equipment
4.1 Gas chromatograph (with nitrogen and phosphorus detectors).
4.2 Headspace autosampler.
4.6 250 µL micro-syringe.
5 Analytical procedures
5.1 Specimen preparation
TAKE 10 g of representative food packaging material, USE a crusher to crush
it or USE scissors to cut it into pieces with a diameter of 0.2 cm or less, MIX it
uniformly, PUT it into a clean container.
5.2 Preparation of test solution
WEIGH 0.5 g (accurate to 0.01 g) of specimen into a headspace flask, ADD 5.0
mL of N,N-dimethylformamide, CAP to seal it immediately, USE a micro-syringe
to add 200 µL of propionitrile standard solution into the headspace flask,
5.3 Instrument reference conditions
5.3.1 Headspace sample injector conditions
Headspace sample injector conditions are listed below.
5.3.2 Gas chromatographic conditions
Gas chromatographic conditions are listed below.
5.4 Calibration solution preparation and calibration curve making
TAKE 5 headspace flasks, respectively ADD 200 µL of propionitrile standard
solution, then ADD acrylonitrile series standard solutions in sequence. At this
time, the acrylonitrile contents in the calibration solution correspond to 2.0 µg,
4.0 µg, 6.0 µg, 8.0 µg, and 10.0 µg, respectively.
5.5 Determination of specimen solution
ADJUST the gas chromatograph to the best working condition. PLACE the
headspace flask containing the liquid to be tested in a headspace sample
injector, TAKE the gas above the liquid and INJECT it into gas chromatograph
for determination, to get the chromatographic peaks corresponding to
acrylonitrile and propionitrile.
6 Expression of analysis results
The content of acrylonitrile in the specimen is calculated in accordance with the
formula (1).
7 Precision
The absolute difference between two independent determinations obtained
under repeatability conditions must not exceed 10% of the arithmetic mean.
8 Others
The method detection limit is 0.1 mg/kg, and the quantitation limit is 0.2 mg/kg.
Determination of acrylonitrile migration
9 Principle
Food contact materials and articles are immersed in food simulants, acrylonitrile
migrates into the soaking liquor. A certain amount of simulated immersion
solution is added to the headspace flask, heated to make the components to
be tested reach gas-liquid equilibrium, then the top air is quantitatively taken for
gas chromatography determination.
10 Reagents and materials
The water used in this method is grade I water specified in GB/T 6682.
Containers and transfer apparatus used in the test shall avoid the use of plastic
materials.
10.1 Reagents
10.1.1 N,N-Dimethylformamide (DMF). Analytically pure, no interference peaks
at the retention times of acrylonitrile and propionitrile.
10.2 Reagent preparation
Water-based, acidic, alcoholic, oil-based food simulants. Operated in
accordance with GB 5009.156.
10.3 Standard substance
10.3.1 Acrylonitrile (C3H3N, CAS No.. 107-13-1). 1000 µg/mL, or a standard
substance that has been certified by the state and granted a standard
substance certificate.
10.3.2 Propionitrile (C2H5CN, CAS No.. 107-12-0). 1000 µg/mL, or a standard
substance that is certified by the state and granted a standard substance
certificate.
10.4 Preparation of acrylonitrile standard solution
Acrylonitrile series standard solution. Respectively PIPETTE 10 µL, 20 µL, 30
µL, 40 µL, and 50 µL of acrylonitrile standard solution into a 10 mL volumetric
flask, respectively ADD N,N-dimethylformamide to dilute it to the mark, MIX it
uniformly(each millimeter is equivalent to 1 µg, 2 µg, 3 µg, 4 µg, and 5 µg of
acrylonitrile), PREPARE it at the day of use.
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.
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