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GB 31604.8-2021: Food safety national standard - Food contact materials and products - Determination of total migration Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB 31604.8: Historical versions
Similar standardsGB 31604.8-2021: Food safety national standard - Food contact materials and products - Determination of total migration---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB31604.8-2021 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Food Contact Materials and Products - Determination of Total Migration Issued on: SEPTEMBER 07, 2021 Implemented on: MARCH 07, 2022 Issued by. National Health Commission of the People's Republic of China; State Administration for Market Regulation. Table of ContentsForeword... 3 1 Scope... 4 Part One -- Determination of total migration in water-based food simulants, chemical alternative solvents... 4 2 Principle... 4 3 Reagents and materials... 4 4 Instruments and equipment... 5 5 Analysis steps... 5 6 Expression of analysis results... 7 7 Precision... 11 Part Two -- Determination of total migration in olive oil... 12 8 Principle... 12 9 Reagents and materials... 12 10 Instruments and equipment... 14 11 Analysis steps... 14 12 Expression of analysis results... 20 13 Precision... 24 Annex A Suitability Judgment... 25 Annex B Confirmation of moisture-sensitive specimens and adjustment of moisture content -- Vacuum drying method... 26 Annex C Confirmation of moisture-sensitive specimens and adjustment of moisture content -- Constant humidity method... 28 Annex D Typical chromatogram... 301 ScopeThis Standard specifies the methods for determination of total migration for food contact materials and products. This Standard is applicable to the determination of total migration for food contact materials and products. Part One -- Determination of total migration in water- based food simulants, chemical alternative solvents2 PrincipleThe specimen uses water-based food simulants and chemical alternative solvents [such as n-hexane, isooctane, 95% (volume fraction) ethanol solution, n-heptane]. Perform migration test under selected migration test conditions. Evaporate and dry the soaking liquid obtained from the migration test. After deducting the corresponding blanks, the total amount of all non-volatile substances migrated from the specimen to water-based food simulants and chemical substitute solvents is obtained.3 Reagents and materialsUnless otherwise specified, the reagents used in this method are analytically pure, and the water is grade two water specified in GB/T 6682. 3.1 Reagents 3.1.1 Absolute ethanol (C2H6O). 3.1.2 Acetic acid (C2H4O2). 3.1.3 Trichloromethane (CHCl3). 3.1.4 N-hexane (C6H14). 3.1.5 Isooctane (C8H18). 3.1.6 95% ethanol. 3.1.7 N-heptane (C7H16).4 Instruments and equipment4.1 Balance. Resolution is 0.1mg. 4.2 Electric heating constant temperature drying oven. 4.3 Electric heating constant temperature water bath or other electric heating equipment.5 Analysis steps5.1 Migration test Food contact materials and products are subjected to migration tests in accordance with the requirements of GB 31604.1 and GB 5009.156. 5.2 Determination of total migration of water-based food simulants and chemical substitute solvents Wash and drain the evaporating dish before use. Dry for 2h in a 100°C±5°C electric heating constant temperature drying oven. Then weigh it after cooling for 0.5h in a desiccator. Repeat drying, cooling, and weighing until constant weight (that is, the difference in mass between the two weighings does not exceed 0.5mg). The last weighed mass is the mass of the empty evaporating dish. 5.3 Determination of trichloromethane extract The determination steps are applicable to food contact materials and products that require the detection of chloroform extracts in the product standard. Add 20mL of chloroform to the residue obtained in 5.2.Wetting the residue. Use the filter paper to filter. Collect the filtrate into an evaporating dish with constant weight. Then use 20mL of chloroform to extract the residue twice respectively. Use a little chloroform to rinse the filter paper. The filtrate is incorporated into the evaporating dish. Steam to dry according to step 5.2.Obtain the mass of the residue extracted with chloroform from the soaking solution for the specimen determination. 5.4 Blank test Treat water-based food simulants, chemical alternative solvents, and chloroform that are not in contact with food contact materials and products according to 5.1, 5.2, and 5.3.Obtain the residue mass of the blank soaking solution and the residue mass of the blank soaking solution extracted with chloroform.6 Expression of analysis results6.1 Total migration calculation 6.1.1 Expressed in mg/dm2 6.1.1.1 Food contact materials and products of non-sealed products When the total migration of food contact materials and products other than sealed products such as lids, gaskets, and connectors (hereinafter referred to as sealing products) is expressed in mg/dm2, it is calculated according to formula (1). Where, 6.1.2 Expressed in mg/kg 6.1.2.1 Food contact materials and products of non-sealed products When the total migration amount of food contact materials and products of non- sealed products is expressed in mg/kg, it is calculated according to formula (3).7 PrecisionWhen the total migration result is ≤ 10.0mg/dm2 or 60.0mg/kg, the difference between the two independent determination results obtained under repeatability conditions and the arithmetic mean shall not exceed 1.0mg/dm2 or 6.0mg/kg. The determination result after applying the correction factor shall also meet this requirement. When the total migration result is > 10.0mg/dm2 or 60.0mg/kg, the difference between the two independent determination results obtained under repeatability conditions and the arithmetic mean shall not exceed 10% of the arithmetic mean. The determination result after applying the correction factor shall also meet this requirement.8 PrincipleThe specimen uses olive oil as a food simulant. The migration test is carried out under the selected conditions. The total migration is determined by the specimen mass reduction method. That is, use the initial mass of the specimen before the migration test to subtract the net mass of the specimen after soaking in olive oil to obtain the mass of non-volatile substances migrated from the specimen. Calculate the corresponding total migration amount according to the formula. The net mass of the specimen after soaking in olive oil is the mass of the specimen when it is taken out of the olive oil minus the mass of olive oil absorbed by the specimen plus the mass of volatile matter. The olive oil absorbed by the specimen is extracted, saponified, and methyl esterified by the Soxhlet extractor to generate fatty acid methyl esters. Use gas chromatography to analyze. Use internal standard method to quantify.9 Reagents and materialsUnless otherwise specified, the reagents used in this method are analytically pure, and the water is grade two water specified in GB/T 6682. 9.1 Reagents 9.1.1 Olive oil. Its mass requirements shall meet the requirements of Annex A of GB 5009.156. 9.1.2 N-Pentane (C5H12). 9.1.3 Absolute ethanol (C2H6O). 9.1.4 N-Heptane (C7H16). Chromatographically pure. 9.1.5 Cyclohexane (C6H12). 9.1.6 Anhydrous sodium sulfate (Na2SO4). 9.1.7 Ether (C4H10O). 9.1.8 Potassium hydroxide (KOH). 9.1.9 Methanol (CH4O). 9.1.10 Boron trifluoride methanol solution. about 150g/L boron trifluoride (BF3). 9.1.11 Sulfuric acid (H2SO4). 9.2 Preparation of reagents 9.2.1 N-pentane-ethanol (95+5) mixed solution. Measure 950mL of n-pentane and mix it with 50mL of absolute ethanol. 9.2.2 Potassium hydroxide-methanol solution (11.0g/L). Weigh 5.5g of (accurate to 0.1g) potassium hydroxide and dissolve it in 500mL of methanol. Mix well. 9.2.3 Saturated sodium sulfate solution. Weigh 50g (accurate to 0.1g) of anhydrous sodium sulfate in a 250mL beaker. Add 100mL of water on the electric hot plate and boil to dissolve. After cooling to room temperature, use a funnel equipped with qualitative filter paper to filter into a breaker. 9.3 Standard product Heptadecanoic acid triglyceride (C54H104O6, CAS number. 2438-40-6). Purity ≥98%, or standard material certified by the country and awarded with a standard material certificate. 9.4 Preparation of standard solution 9.4.1 Internal standard solution (2.0mg/mL) Accurately weigh 1.0g (accurate to 0.1mg) of heptadecanoic acid triglyceride. Place in a 100mL beaker. Add cyclohexane to dissolve. Transfer to a 500mL volumetric flask. Wash the beaker 3 times with cyclohexane. The washing liquid is combined into the volumetric flask. Use cyclohexane to set volume. Store in a refrigerator at 4°C. The validity period is 1 month. 9.4.2 Olive oil standard stock solution (100mg/mL) Weigh 5.0g of blank olive oil obtained from migration test (accurate to 0.1mg). Place in a 50mL beaker. Add n-heptane to dissolve. Transfer to a 50mL volumetric flask. Wash the beaker 3 times with n-heptane. The washing liquid is combined into the volumetric flask. Use N-heptane to set volume. Prepare it when it is required. 9.5 Materials 9.5.1 Heating plate. 9.5.2 Airtight moisture content adjustment container. Such as glass dryer. 9.5.3 Filter membrane. Organic phase, 0.22μm. 9.5.4 Filter paper. Qualitative filter paper, fast. 9.5.5 Dust-free wipe paper. 9.5.6 Glass fiber filter cartridge.10 Instruments and equipment10.1 Gas chromatograph. Equipped with a hydrogen flame ionization detector (FID). 10.2 Analytical balance. Resolutions are 0.1mg, 0.1g. 10.3 Soxhlet extractor. 10.4 Low temperature circulating condensate pump. 10.5 Electric heating constant temperature water bath. 10.6 Rotary evaporator. 10.7 Vacuum drying oven. 10.8 Humidity chamber.11 Analysis steps11.1 Specimen preparation Food contact materials and products are prepared according to the requirements of GB 31604.1 and GB 5009.156 for migration test. The specimen preparation area of total immersion method and filling method shall be ≥1dm2. The area of the specimen in the test cell method is calculated based on the actual area of the specimen in contact with the food simulant. The specimen preparation area of bagging method shall be ≥2dm2.Each specimen can be prepared from multiple products. The number of specimens is determined according to the following purposes. a) Migration test. At least 3 specimens of disposable products; At least 3 specimens per set of specimens for repeated use of products; b) Volatile matter determination. 2 specimens; c) Suitability judgment (see Annex A). 2 specimens; d) Surface area determination. 1 specimen; e) Confirmation of moisture sensitivity. 2 specimens. 11.2 Suitability Judgment Take 2 specimens to determine the suitability of the method according to the steps described in Annex A. If the previous test has confirmed the suitability of the method, it can omit the steps in Annex A. 11.3 Weighing of the initial mass of the specimen Determine whether the specimen is moisture sensitive according to the steps described in Annex B or Annex C. If the previous test has confirmed that the specimen is a non-moisture-sensitive specimen, it can omit the steps in Annex B or Annex C. If the specimen is a non-moisture sensitive specimen, directly weigh the initial mass. If the specimen is moisture sensitive, after adjusting the moisture content according to the steps described in the relevant appendix, the initial mass of the specimen is obtained. If the specimen adopts the steps described in Annex C to adjust the moisture content and cannot reach a constant weight within 5d, use Annex B to adjust the moisture content. 11.4 Migration test The migration test of food contact materials and products shall be conducted in accordance with the requirements of GB 31604.1 and GB 5009.156.For reusable products, test on 3 sets of specimens prepared from the same batch of test specimens. Each group of specimens differs only in the migration test time. The migration test time of the first group of specimens is the migration test time determined according to the requirements of relevant standards. The migration test time of the second group of specimens is twice that of the first group. The migration test time of the third group of specimens is 3 times that of the first group. The number of parallel specimens for migration test should meet the requirements of 11.1a). 11.5 Weighing the final mass of the specimen Remove the specimen from the olive oil as soon as possible after the migration test is completed. Cool to room temperature. Place the specimen between two filter papers or dust-free wipes. Lightly press it. Suck off the olive oil on the surface of the specimen. Repeat the pressing steps until no oil spots appear on the paper. No paper fibers shall remain on the surface of the specimen. For non-moisture sensitive specimens, directly weigh the final mass. After adjusting the moisture content of the moisture-sensitive specimen in the same way as in 11.3, weigh the final mass. 11.6 Determination of the volatile matter of the specimen Prepare 2 parallel specimens according to the steps described in 11.1.Obtain the initial mass of the specimen according to the steps described in 11.3.Except that no olive oil is added, carry out the migration test according to the steps described in 11.4.For non-moisture sensitive specimens, directly weigh the final mass. After adjusting the moisture content of the moisture-sensitive specimen in the same way as in 11.3, weigh the final mass. The mass of volatile matter per unit area of each parallel specimen is calculated by dividing the difference between the initial mass and the final mass of the specimen by the corresponding sampling area. If the moisture content of the specimen is adjusted according to the steps described in Annex B, this step can be omitted. 11.7 Blank test Follow the steps in 11.4 to dispose of olive oil that is not in contact with food contact materials and products. Use it to prepare olive oil standard stock solution. 11.8 Determination of the absorption of olive oil by the specimen 11.8.1 The first extraction of olive oil The extraction solvent is selected according to the main polymer material of the food contact surface of the food contact materials and products. When the main material is the specimen of non-polar polymer (such as polyethylene, polypropylene), use N-pentane. When the main material is a specimen of polar polymer (such as polyethylene terephthalate), use a mixed solution of n- pentane-ethanol (95+5). Add 10.0mL of internal standard solution (2.0mg/mL) and extraction solvent to the collection bottle of the Soxhlet extractor. Add zeolite or glass beads to prevent explosion boiling. Cut the specimen into suitable size. Wrap it with qualitative filter paper or put it in a glass fiber sleeve barrel (including specimen debris, particles generated during the cutting process). Put into Soxhlet extractor. Perform reflux extraction for 7h~8h. Cycle at least 6 times per hour. Make sure that the specimen is completely immersed in the solvent and kept separate from each other during each cycle. 11.8.2 The first methyl esterification of olive oil 11.8.2.1 Transfer of extract The obtained extraction solution is evaporated to about 10mL with a rotary evaporator or distillation device and transferred to a 50mL flask. Wash the collection bottle with extraction solvent 3 times. Combine the detergent that have been washed for 3 times into the flask. Evaporate to dryness on a rotary evaporator.12 Expression of analysis results12.1 Expressed in mg/dm2 12.1.1 Food contact materials and products of non-sealed products When the total migration amount of food contact materials and products of non- sealed products is expressed in mg/dm2, it is calculated according to formula (8). 12.3 Expressed in mg/piece The total migration amount of food contact materials and products of sealed products is expressed in mg/piece. Calculate according to formula (12). The migration test method used and the area of contact between a single sealed product and the food simulant in the migration test shall be indicated. 12.4 Correction of results When GB 31604.1 specifies the correction factor for fat-containing food simulants, the determination results shall be divided by the corresponding correction factor. 12.5 Expression of results The calculation result of total migration is the arithmetic mean of 3 parallel determination results. The calculation result is accurate to one decimal place.13 PrecisionWhen the total migration result is ≤ 10.0mg/dm2 or 60.0mg/kg, the difference between the three independent determination results obtained under repeatability conditions and the arithmetic mean shall not exceed 3.0mg/dm2 or 20.0mg/kg. The determination result after applying the correction factor shall also meet this requirement. When the total migration result is > 10.0mg/dm2 or 60.0mg/kg, the difference between the three independent determination results obtained under repeatability conditions and the arithmetic mean shall not exceed 30% of the arithmetic mean. The determination result after applying the correction factor shall also meet this requirement. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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