Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces GB/T 23296.17-2009 Food Contact Materials - Polymer - Determination of 1 2-diaminoethane and 1 6-diaminohexane in Food Simulants - Gas Chromatography
The following changes have been made with respect to GB/T 23296.17-2009 (the previous edition):
——this standard is renamed as National Food Safety Standard - Food Contact Materials and Articles - Determination of Migration of Ethylenediamine and Hexamethylene Diamine.
National Food Safety Standard
Food Contact Materials and Articles
Determination of Migration of Ethylenediamine and Hexamethylene Diamine
1 Scope
This standard specifies the determination method of gas chromatography for the migration of ethylenediamine and hexamethylene diamine in food contact materials and articles.
This standard is applicable to the determination of migration of ethylenediamine and hexamethylene diamine in food contact materials and articles.
2 Principle
With the ethyl chloroformate as the derivatization reagent, derive the ethylenediamine and hexamethylene diamine in food simulants and transform them into corresponding derived products of dicarbamate ethyl ester, separate by gas chromatographic column, and detect by hydrogen flame ionization detector. Carry out the quantitative determination by internal standard method with 1,3-propylene diamine as the internal standard sbustance.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Class-I water (defined in GB/T 6682) are adopted for the purpose of this method. Containers and transfer appliances in test shall not be made of plastic materials.
3.1 Reagents
3.1.1 Ethyl chloroformate (C3H5ClO2): with purity >97%.
3.1.2 Glacial acetic acid (C2H4O2).
3.1.3 Absolute ethanol(C2H6O).
3.1.4 Toluene(C7H8).
3.1.5 Ethyl ether (C4H10O).
3.1.6 Isooctane (C8H18).
3.1.7 Anhydrous sodium sulfate (Na2SO4).
3.1.8 Sodium hydroxide (NaOH).
3.1.9 Ammonia: with concentration of 25% (mass fraction).
3.1.10 Reagents required for preparation of water-based, acidic, alcoholic and oil-based food simulants: in accordance with the requirements of GB 31604.1.
3.2 Preparation of reagents
3.2.1 Water-based, acidic, alcoholic and oil-based food simulants: prepare according to GB 5009.156.
3.2.2 Ammonia solution (3%, volume fraction): add 200 mL water and 30 mL ammonia solution (25%) into a 250 mL conical flask and mix uniformly.
3.2.3 Sodium hydroxide solution (5 mol/L): weigh 50.0 g (accurate to 0.1 g) sodium hydroxide, put into a 250mL volumetric flask and scale the volume with water.
3.2.4 Acetic acid solution (4%, mass fraction): weigh 40 g (accurate to 0.1 g) glacial acetic acid, put into a 1 L volumetric flask and scale the volume with water.
3.2.5 Ethanol solution (10%, volume fraction): measure 100 mL absolute ethanol, put into a 1 L volumetric flask and scale the volume with water.
3.2.6 Ethanol solution (95%, volume fraction): measure 475 mL absolute ethanol, put into a 500 mL volumetric flask and scale the volume with water.
3.3 Standard products
3.3.1 Ethylenediamine (C2H8N2, CAS No.: 107-15-3): with purity>99% or the reference material approved and awarded with reference material certificate by the State.
3.3.2 Hexamethylene diamine (C6H16N2, CAS No.: 124-09-4): with purity >99% or the reference material approved and awarded with reference material certificate by the State.
3.3.3 1,3-propylene diamine (C3H10N2, CAS No.: 78-90-0): with purity>99%, or the reference material approved and awarded with reference material certificate by the State.
3.4 Preparation of standard solutions
3.4.1 Water-based ethylenediamine stock solution (1,000 mg/L): accurately weigh 50 mg (accurate to 0.1 mg) ethylenediamine, put into a 50 mL volumetric flask and scale the volume with water.
3.4.2 Water-based hexamethylene diamine stock solution (500 mg/L): accurately weigh 25 mg (accurate to 0.1 mg) hexamethylene diamine, put into a 50 mL volumetric flask and scale the volume with water.
3.4.3 Water-based propylene diamine stock solution (500 mg/L): accurately weigh 25 mg (accurate to 0.1 mg) propylene diamine, put into a 50 mL volumetric flask and scale the volume with water.
3.4.4 Toluene-based ethylenediamine stock solution (1,000 mg/L): accurately weigh 50 mg (accurate to 0.1 mg) ethylenediamine, put into a 50 mL volumetric flask and scale the volume with toluene.
3.4.5 Toluene-based hexamethylene diamine stock solution (500 mg/L): accurately weigh 25 mg hexamethylene diamine (accurate to 0.1 mg), put into a 50 mL volumetric flask and scale the volume with toluene.
3.4.6 Toluene-based propylene diamine stock solution (500 mg/L): accurately weigh 25 mg (accurate to 0.1 mg) propylene diamine, put into a 50 mL volumetric flask and scale the volume with toluene.
The stock solutions prepared can be kept sealed in dark places at 5℃~20℃ and be valid for 3 months.
3.5 Utensils and Materials
3.5.1 Glass bottle: 2 mL, 10 mL; with its cap equipped with PTFE butyl rubber or silicone rubber sealing gasket.
3.5.2 Volumetric flask: 50 mL.
3.5.3 Microinjector: 10 μL and 25 μL.
3.5.4 Oscillator.
4 Instruments and Apparatus
4.1 Gas chromatograph: equipped with hydrogen flame ionization detector and automatic data analysis software.
4.2 Analytical balance: with sensibility of 0.0001 g and 0.01 g.
5 Analysis Steps
5.1 Preparation of standard working solutions and specimens
5.1.1 Preparation of standard working solutions
5.1.1.1 Water-based, acidic and alcoholic food simulants and ethanol (95%, volume fraction) standard working solutions
Add 1 mL water and 10 μL water-based propylene diamine stock solution into seven 10 mL glass bottles, add 0 μL, 1 μL, 2 μL, 3 μL, 5 μL, 12 μL and 24 μL water-based ethylenediamine stock solutions and 0 μL, 1 μL, 2 μL, 4 μL, 6 μL, 8 μL and 10 μL water-based hexamethylene diamine stock solutions in sequence, place the cap for sealing, and mix uniformly. The concentrations of ethylenediamine in water as obtained are 0.00 mg/L, 1.00 mg/L, 2.00 mg/L, 3.00 mg/L, 5.00 mg/L, 12.0 mg/L and 24.0 mg/L respectively, while those of hexamethylene diamine are 0.00 mg/L, 0.500 mg/L, 1.00 mg/L, 2.00 mg/L, 3.00 mg/L, 4.00 mg/L and 5.00 mg/L respectively. In the similar way, prepare ethylenediamine and hexamethylene diamine standard working solutions with the same concentration series with acidic and alcoholic food simulants and ethanol solution (95%, volume fraction) respectively.
Foreword i
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Apparatus
5 Analysis Steps
6 Expression of Analysis Results
7 Accuracy
8 Other
Annex A Chromatogram of Ethylenediamine and Hexamethylene Diamine Derivatives in Food Simulant Standard Solution
