GB 31604.26-2016 National Food Safety Standard - Food Contact Materials and Articles -Determination of Epichlorohydrin and Determination of Migration (English Version)
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 23296.7-2009 Food Contact Materials - Determination of Epichlorohydrin in Plastics - High Performance Liquid Chromatography and SN/T 2897-2011 Food Contact Materials for Export - Metal Materials - Determination of Epichlorohydrin in Coating - Gas chromatography.
The following main changes have been made with respect to 23296.7-2009 (the previous edition):
——This standard is renamed as National Food Safety Standard - Food Contact Materials and Articles -Determination of Epichlorohydrin and Determination of Migration;
——Application scope is added;
——Sample preparation method for coating is modified;
——Examination method for migration of epichlorohydrin in food contact materials and articles is added.
National Food Safety Standard
Food Contact Materials and Articles
Determination of Epichlorohydrin and Determination of Migration
1 Scope
This standard specifies the determination method of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board) and determination method of migration.
This standard is applicable to determination method of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board) and determination method of migration of epichlorohydrin, therein, high performance liquid chromatography is applicable to determination of epichlorohydrin in food contact materials and articles (plastic, paint and paper product) while gas chromatography-mass spectrometry is applicable to determination of migration of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board).
Determination of Epichlorohydrin
2 Principle
Extract epichlorohydrin in the specimen with 1,4-dioxane, distill extracting solution by micro-distillation apparatus, derive epichlorohydrin in distillate, separate derivative by liquid chromatography, determine content of epichlorohydrin derivative by fluorescence detector and convert into content of epichlorohydrin in the specimen. Carry out quantitative determination by external standard method.
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.
3.1 Reagents
3.1.1 Acetonitrile (C2H3N): chromatographically pure.
3.1.2 9,10-Dimethoxyanthracene-2-Sulfonicacidsodiumsalt (C16H13NaO5S), i.e DAS-Na.
3.1.3 1,4-dioxane (C4H8O2): with purity>99% and water content˂0.01%.
3.1.4 Methanol (CH4O): chromatographically pure.
3.1.5 Strong-acid cation exchange resin.
3.1.6 Nitrogen: with purity≥99.9%.
3.1.7 Ice block.
3.2 Preparation of reagents
3.2.1 Methanol solution (80%, volume fraction)
Measure 400 mL methanol into a 500 mL volumetric flask and scale the volume with water.
3.2.2 9,10-Dimethoxyanthracene-2-sulphonicacid reagent (DAS reagent)
Activate abt. 50 g pretreated strong-acid cation exchange resin with 200 mL methanol solution (80%, volume fraction) and fill glass column with inside diameter of 1 cm with resin until height of resin is abt. 20 cm for standby. Weigh 100 mg DAS-Na into beaker containing 20 mL methanol in advance, heat to dissolve and pass all solution through strong-acid cation exchange resin in 2~3 times. Elute with methanol to make flow rate of effluent about 0.5 mL/min, collect eluent with pH value of 1~2 until pH value starts to rise. Blow to dry the eluent with nitrogen blower and obtain DAS reagent. Keep it in dark place, with the valid period of a year.
3.2.3 DAS-acetonitrile solution (5 mg/mL)
Weigh 20 mg (accurate to 0.1 mg) DAS reagent and dissolve in 4 mL acetonitrile. Prepare immediately before use and keep it in dark place.
3.3 Standard product
Epichlorohydrin (C3H5ClO,CAS No.: 106-89-8), with purity>99%, or reference material approved and awarded with reference material certificate by the State.
3.4 Preparation of standard solution
3.4.1 Epichlorohydrin standard stock solution (1 mg/mL)
Weigh 100 mg (accurate to 0.1 mg) epichlorohydrin into 100 mL volumetric flask and scale the volume with 1,4-dioxane. Seal and preserve it at dark place at -20℃~20℃, with the valid period of 3 months.
3.4.2 Epichlorohydrin standard working solution (40 μg/mL)
Accurately transfer 2.0 mL epichlorohydrin standard stock solution (1 mg/mL) into 50 mL volumetric flask and scale the volume with 1,4-dioxane.
3.4.3 Epichlorohydrin standard intermediate solution
Respectively transfer 0.0 mL, 0.5 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL and 5.0 mL epichlorohydrin standard working solution (40 μg/mL) into seven 25mL volumetric flasks and scale the volume with 1,4-dioxane. The concentrations of the standard intermediate solution are: 0 μg/mL, 0.8 μg/mL, 1.6 μg/mL, 3.2 μg/mL, 4.8 μg/mL and 6.4 μg/mL and 8.0 μg/mL respectively.
3.4.4 Epichlorohydrin standard working solution
Respectively transfer 10.0 mL 1,4-dioxane into 7 sample bottles, accurately add 100 μL epichlorohydrin standard intermediate solution respectively, add magnetic stirring bar and seal with isolation pad and aluminum cap. Mark the sample bottle as Ab. Concentrations of epichlorohydrin standard working solution are 0 μg/L, 8 μg/L, 16 μg/L, 32 μg/L, 48 μg/L, 64 μg/L and 80 μg/L respectively.
4 Instruments and Apparatus
4.1 High performance liquid chromatograph: equipped with 20 μL quantitative loop and fluorescence detector.
4.2 Analytical balance: with sensitivity of 1 mg and 0.1 mg.
4.3 Micro-distillation apparatus (as shown in A.1).
4.4 Nitrogen blower.
4.5 Sample bottle: 20mL; equipped with aluminum cap and butyl rubber or silicone resin rubber isolation pad whose side contacting sample shall be coated with polytetrafluoroethylene.
Note: appropriate sample bottle, if not any, may be replaced by headspace bottle.
4.6 Pipette: 50 μL and 100μL.
4.7 Analytical balance: with sensibility of 0.1 mg.
4.8 Microporous filter membrane: 0.22 μm.
Note: filter membrane used shall not generate adsorption on epichlorohydrin derivative.
4.9 Volumetric flask.
5 Analysis Steps
5.1 Preparation of specimen
When testing samples of plastic products and paper and board contacting with foods, cut samples into several scraps with area of 2 dm2 and randomly take two pieces as parallel specimen. Cut 2 dm2 scraps into fragments with area of 1 cm2 for standby. Slightly scrape off abt. 0.2 g coating samples for standby.
5.2 Preparation of specimen solution
5.2.1 Preparation of plastic and paper product specimen extracting solution
Weigh 0.50 g (accurate to 0.1 mg) standby to-be-tested plastic or paper product, immerge into 50.0 mL 1,4-dioxane and seal. Extract for 6 h under ambient temperature. Transfer 10.0 mL extracting solution into 20 mL sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark headspace bottle as As.
5.2.2 Preparation of coating extracting solution
Weigh 0.15 g (accurate to 0.1 mg) standby coating sample, immerge into 15.0 mL 1,4-dioxane and seal. Extract for 6 h under ambient temperature. Transfer 10.0 mL extracting solution into the sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark sample bottle as As.
Note 1: This standard specifies determination method for content of epichlorohydrin in plastic products, paper and board product and coating product, and it is expected to be applicable to all food contact materials and articles containing epichlorohydrin.
Note 2: if coating of specimen in plastic package or container is thicker, temperature or extraction time shall be increased. and all extraction process shall be conducted in closed environment to prevent epichlorohydrin from escaping.
5.3 Preparation of blank solution
Transfer 10.0 mL 1,4-dioxane not in contact with plastic, paper product or coating sample into 20 mL sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark sample bottle as A0.
5.4 Distillation of 1,4-dioxane extracting solution
Distill 1,4-dioxane extracting solution by micro-distillation apparatus in Figure A.1 and collect part of distillate. Bottle A in Figure A.1 refers to sample bottles in 5.2.1, 5.2.2, 5.3 and 3.4.4, which contain 10 mL specimen extracting solution, blank solution and standard working solution respectively.
Separately take a 20 mL sample bottle, mark at volume of 3 mL and seal with isolation pad and aluminum cap. Weigh (accurate to 0.1 mg) sealed sample bottle and mark as bottle B.
As shown in Figure A.1, connect bottle A and bottle B with stainless steel tube covered with polytetrafluoroethylene on external layer; steel tube shall penetrate into bottle A 1cm~2 cm and bottle B 3 cm~4 cm. To avoid pipe orifice blocking, one orifice shall be pierced in advance on bottle stopper of sample bottle to allow steel tube rapidly penetrate into the bottle. Meanwhile, insert injector needle on cap of bottle B to avoid overlarge pressure in the bottle.
Place bottle A at heating plate and bottle B at beaker containing ice water mixture. Heat bottle A to make 1,4-dioxane extracting solution boil, continuously and slowly heat to make 1,4-dioxane extracting solution in bottle A distill to bottle B until level of distillate in bottle B reach marked place of 3 mL. Remove bottle A from heating plate and injector needle and stainless steel tube in bottle B. Carefully dry bottle B with filter paper. Re-weigh (accurate to 0.1 mg) bottle B and calculate volume of distillate according to difference between weighed values and density of 1,4-dioxane.
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
9 Principle
10 Reagents and Materials
11 Instruments and Apparatus
12 Analysis Steps
13 Expression of Analysis Results
14 Accuracy
15 Other
Annex A Micro-distillation Apparatus
Annex B Liquid Chromatogram for DAS Derivative of Epichlorohydrin
Annex C
GB 31604.26-2016 National Food Safety Standard - Food Contact Materials and Articles -Determination of Epichlorohydrin and Determination of Migration (English Version)
Standard No.
GB 31604.26-2016
Status
valid
Language
English
File Format
PDF
Word Count
5000 words
Price(USD)
80.0
Implemented on
2017-4-19
Delivery
via email in 1 business day
Detail of GB 31604.26-2016
Standard No.
GB 31604.26-2016
English Name
National Food Safety Standard - Food Contact Materials and Articles -Determination of Epichlorohydrin and Determination of Migration
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 23296.7-2009 Food Contact Materials - Determination of Epichlorohydrin in Plastics - High Performance Liquid Chromatography and SN/T 2897-2011 Food Contact Materials for Export - Metal Materials - Determination of Epichlorohydrin in Coating - Gas chromatography.
The following main changes have been made with respect to 23296.7-2009 (the previous edition):
——This standard is renamed as National Food Safety Standard - Food Contact Materials and Articles -Determination of Epichlorohydrin and Determination of Migration;
——Application scope is added;
——Sample preparation method for coating is modified;
——Examination method for migration of epichlorohydrin in food contact materials and articles is added.
National Food Safety Standard
Food Contact Materials and Articles
Determination of Epichlorohydrin and Determination of Migration
1 Scope
This standard specifies the determination method of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board) and determination method of migration.
This standard is applicable to determination method of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board) and determination method of migration of epichlorohydrin, therein, high performance liquid chromatography is applicable to determination of epichlorohydrin in food contact materials and articles (plastic, paint and paper product) while gas chromatography-mass spectrometry is applicable to determination of migration of epichlorohydrin in food contact materials and articles (plastic, paint, paper and board).
Determination of Epichlorohydrin
2 Principle
Extract epichlorohydrin in the specimen with 1,4-dioxane, distill extracting solution by micro-distillation apparatus, derive epichlorohydrin in distillate, separate derivative by liquid chromatography, determine content of epichlorohydrin derivative by fluorescence detector and convert into content of epichlorohydrin in the specimen. Carry out quantitative determination by external standard method.
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.
3.1 Reagents
3.1.1 Acetonitrile (C2H3N): chromatographically pure.
3.1.2 9,10-Dimethoxyanthracene-2-Sulfonicacidsodiumsalt (C16H13NaO5S), i.e DAS-Na.
3.1.3 1,4-dioxane (C4H8O2): with purity>99% and water content˂0.01%.
3.1.4 Methanol (CH4O): chromatographically pure.
3.1.5 Strong-acid cation exchange resin.
3.1.6 Nitrogen: with purity≥99.9%.
3.1.7 Ice block.
3.2 Preparation of reagents
3.2.1 Methanol solution (80%, volume fraction)
Measure 400 mL methanol into a 500 mL volumetric flask and scale the volume with water.
3.2.2 9,10-Dimethoxyanthracene-2-sulphonicacid reagent (DAS reagent)
Activate abt. 50 g pretreated strong-acid cation exchange resin with 200 mL methanol solution (80%, volume fraction) and fill glass column with inside diameter of 1 cm with resin until height of resin is abt. 20 cm for standby. Weigh 100 mg DAS-Na into beaker containing 20 mL methanol in advance, heat to dissolve and pass all solution through strong-acid cation exchange resin in 2~3 times. Elute with methanol to make flow rate of effluent about 0.5 mL/min, collect eluent with pH value of 1~2 until pH value starts to rise. Blow to dry the eluent with nitrogen blower and obtain DAS reagent. Keep it in dark place, with the valid period of a year.
3.2.3 DAS-acetonitrile solution (5 mg/mL)
Weigh 20 mg (accurate to 0.1 mg) DAS reagent and dissolve in 4 mL acetonitrile. Prepare immediately before use and keep it in dark place.
3.3 Standard product
Epichlorohydrin (C3H5ClO,CAS No.: 106-89-8), with purity>99%, or reference material approved and awarded with reference material certificate by the State.
3.4 Preparation of standard solution
3.4.1 Epichlorohydrin standard stock solution (1 mg/mL)
Weigh 100 mg (accurate to 0.1 mg) epichlorohydrin into 100 mL volumetric flask and scale the volume with 1,4-dioxane. Seal and preserve it at dark place at -20℃~20℃, with the valid period of 3 months.
3.4.2 Epichlorohydrin standard working solution (40 μg/mL)
Accurately transfer 2.0 mL epichlorohydrin standard stock solution (1 mg/mL) into 50 mL volumetric flask and scale the volume with 1,4-dioxane.
3.4.3 Epichlorohydrin standard intermediate solution
Respectively transfer 0.0 mL, 0.5 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL and 5.0 mL epichlorohydrin standard working solution (40 μg/mL) into seven 25mL volumetric flasks and scale the volume with 1,4-dioxane. The concentrations of the standard intermediate solution are: 0 μg/mL, 0.8 μg/mL, 1.6 μg/mL, 3.2 μg/mL, 4.8 μg/mL and 6.4 μg/mL and 8.0 μg/mL respectively.
3.4.4 Epichlorohydrin standard working solution
Respectively transfer 10.0 mL 1,4-dioxane into 7 sample bottles, accurately add 100 μL epichlorohydrin standard intermediate solution respectively, add magnetic stirring bar and seal with isolation pad and aluminum cap. Mark the sample bottle as Ab. Concentrations of epichlorohydrin standard working solution are 0 μg/L, 8 μg/L, 16 μg/L, 32 μg/L, 48 μg/L, 64 μg/L and 80 μg/L respectively.
4 Instruments and Apparatus
4.1 High performance liquid chromatograph: equipped with 20 μL quantitative loop and fluorescence detector.
4.2 Analytical balance: with sensitivity of 1 mg and 0.1 mg.
4.3 Micro-distillation apparatus (as shown in A.1).
4.4 Nitrogen blower.
4.5 Sample bottle: 20mL; equipped with aluminum cap and butyl rubber or silicone resin rubber isolation pad whose side contacting sample shall be coated with polytetrafluoroethylene.
Note: appropriate sample bottle, if not any, may be replaced by headspace bottle.
4.6 Pipette: 50 μL and 100μL.
4.7 Analytical balance: with sensibility of 0.1 mg.
4.8 Microporous filter membrane: 0.22 μm.
Note: filter membrane used shall not generate adsorption on epichlorohydrin derivative.
4.9 Volumetric flask.
5 Analysis Steps
5.1 Preparation of specimen
When testing samples of plastic products and paper and board contacting with foods, cut samples into several scraps with area of 2 dm2 and randomly take two pieces as parallel specimen. Cut 2 dm2 scraps into fragments with area of 1 cm2 for standby. Slightly scrape off abt. 0.2 g coating samples for standby.
5.2 Preparation of specimen solution
5.2.1 Preparation of plastic and paper product specimen extracting solution
Weigh 0.50 g (accurate to 0.1 mg) standby to-be-tested plastic or paper product, immerge into 50.0 mL 1,4-dioxane and seal. Extract for 6 h under ambient temperature. Transfer 10.0 mL extracting solution into 20 mL sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark headspace bottle as As.
5.2.2 Preparation of coating extracting solution
Weigh 0.15 g (accurate to 0.1 mg) standby coating sample, immerge into 15.0 mL 1,4-dioxane and seal. Extract for 6 h under ambient temperature. Transfer 10.0 mL extracting solution into the sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark sample bottle as As.
Note 1: This standard specifies determination method for content of epichlorohydrin in plastic products, paper and board product and coating product, and it is expected to be applicable to all food contact materials and articles containing epichlorohydrin.
Note 2: if coating of specimen in plastic package or container is thicker, temperature or extraction time shall be increased. and all extraction process shall be conducted in closed environment to prevent epichlorohydrin from escaping.
5.3 Preparation of blank solution
Transfer 10.0 mL 1,4-dioxane not in contact with plastic, paper product or coating sample into 20 mL sample bottle, add magnetic stirring bar, seal with isolation pad and aluminum cap and mark sample bottle as A0.
5.4 Distillation of 1,4-dioxane extracting solution
Distill 1,4-dioxane extracting solution by micro-distillation apparatus in Figure A.1 and collect part of distillate. Bottle A in Figure A.1 refers to sample bottles in 5.2.1, 5.2.2, 5.3 and 3.4.4, which contain 10 mL specimen extracting solution, blank solution and standard working solution respectively.
Separately take a 20 mL sample bottle, mark at volume of 3 mL and seal with isolation pad and aluminum cap. Weigh (accurate to 0.1 mg) sealed sample bottle and mark as bottle B.
As shown in Figure A.1, connect bottle A and bottle B with stainless steel tube covered with polytetrafluoroethylene on external layer; steel tube shall penetrate into bottle A 1cm~2 cm and bottle B 3 cm~4 cm. To avoid pipe orifice blocking, one orifice shall be pierced in advance on bottle stopper of sample bottle to allow steel tube rapidly penetrate into the bottle. Meanwhile, insert injector needle on cap of bottle B to avoid overlarge pressure in the bottle.
Place bottle A at heating plate and bottle B at beaker containing ice water mixture. Heat bottle A to make 1,4-dioxane extracting solution boil, continuously and slowly heat to make 1,4-dioxane extracting solution in bottle A distill to bottle B until level of distillate in bottle B reach marked place of 3 mL. Remove bottle A from heating plate and injector needle and stainless steel tube in bottle B. Carefully dry bottle B with filter paper. Re-weigh (accurate to 0.1 mg) bottle B and calculate volume of distillate according to difference between weighed values and density of 1,4-dioxane.
Contents of GB 31604.26-2016
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
9 Principle
10 Reagents and Materials
11 Instruments and Apparatus
12 Analysis Steps
13 Expression of Analysis Results
14 Accuracy
15 Other
Annex A Micro-distillation Apparatus
Annex B Liquid Chromatogram for DAS Derivative of Epichlorohydrin
Annex C
