This standard specifies the general rules for immersion test methods for food packaging materials and their products. This standard is applicable to the pretreatment of physical and chemical test samples such as various food utensils, containers, food packaging materials, pipes, samples, resin pellets, and plates made of plastics, ceramics, enamel, aluminum, stainless steel, rubber, etc. GB/T 5009.156-2003 General rules for immersion test methods for food packaging materials and their products GB/T5009.156-2003 standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.156—2003
Replaces GB/T17409—1998
General principle for the determination ofmigration of packaging materials andtheir products
Promulgated on August 11, 2003
Ministry of Health of the People's Republic of China
Administrative Committee of Standardization of the People's Republic of China
Implementation on January 1, 2004
GB/T5009.156—2003
This standard replaces CB/T17409—1998 "General principle for the determination ofmigration of packaging materials and their products". This standard modifies the structure of the original standard in accordance with GB/T20001.4-2001 "Standard Abbreviation Rules Part 4: Chemical Analysis Methods".
This standard is proposed and managed by the Ministry of Health of the People's Republic of China. Appendix A and Appendix B of this standard are normative appendices. The responsible drafting units of this standard are Shanghai Municipal Health and Epidemic Prevention Station, Shanghai Nanshi District Health and Epidemic Prevention Station, Jiangxi Provincial Health and Epidemic Prevention Station, and Tianjin Municipal Health and Epidemic Prevention Station.
The main drafters of this standard are Shen Wen, Cheng Kaitai, Liu Cuiying, Yang Xiaomei, and Zhu Huifen. The original standard was first issued in 1998, and this is the first revision. 303
GB/T5009.156—2003
After years of standard-making work by researchers, a series of standards for the hygienic inspection methods of food packaging materials and their products have gradually been formed in my country. Due to objective reasons, there are still many problems in each immersion test. To this end, this principle has been formulated based on reference to relevant domestic and foreign information, in order to streamline and supplement, so that the operating procedures can be standardized and unified, and as close as possible to international standards, so that the monitoring operation is simple and scientific.
1 Scope
General rules for immersion test methods for food packaging materials and their products
This standard specifies the general rules for immersion test methods for food packaging materials and their products. GB/T5009.156-2003
This standard applies to the pretreatment of physical and chemical test samples of various food utensils, containers, food packaging materials made of plastics, ceramics, sugar porcelain, aluminum, stainless steel, rubber, etc., as well as pipes, samples, resin pellets, plates, etc. 2 Definitions
The following definitions apply to this standard.
2.1 Food utensils
Cooking spoons, cutting boards and tableware used for food processing, such as spoons, chopsticks, knives, forks, etc. 2.2 Food containers
Utensils for holding food, including cooking containers, storage containers, etc. 2.2.1 Hollow products are products whose depth from the lowest point inside to the overflow surface when filled with liquid is greater than 25mm when placed in a horizontal position, such as bowls, pots, and bottles. Hollow products can be divided into the following two types according to their capacity: a) Large hollow products: those with a capacity greater than or equal to 1.1L and less than 3L; b) Small hollow products: those with a capacity less than 1.1L. 2.2.2 Flat products: products whose depth from the lowest point inside to the overflow surface when filled with liquid is less than or equal to 25mm when placed in a horizontal position, such as plates and dishes.
2.2.3 Storage containers: products with a capacity greater than or equal to 3L. 3 Sampling methods
Product name, production date, batch number, and manufacturer should be recorded during sampling. The sampled products should be complete, stable, without deformation, without incomplete images, consistent in capacity, and without other points that affect the test results. The number of samples should reflect the quality of the product and meet the requirements of the test items for the sample quantity. One set of samples is used for inspection, re-inspection, and reference or arbitration (see Appendix A). 4 Preparation of samples
4.1 Determination of the volume of hollow products
Place the hollow product on a horizontal table, use a measuring cylinder to fill it with water to 5mm from the upper edge (overflow surface), and record its volume (V) with an accuracy of ±2%.
The volume of the inner wall coating of the can is determined in the same way as that of the hollow product. 4.2 Determination of the reference area of ​​flat products
Put the flat product upside down on a standard calculation paper with square millimeters, draw an outline along the edge of the product, and record this reference area (A), expressed in square centimeters (cm). For round flat products, you can measure its diameter (D, expressed in centimeters) and calculate its reference area according to formula (1). S
S——area, cm [The meanings of formula (2) to (8) are the same] D—diameter cm [The meanings of formula (2) to (8) are the same] * (1)
GB/T5009.156-2003
Distance from immersion liquid to edge, cm
4.3 For products that cannot hold liquids, i.e., flat products that cannot leave a distance of 5mm from the liquid surface to the upper edge when holding liquids, the area measurement is the same as the above flat products.
4.4 Examples of area measurement methods for products of different shapes 4.4.1 Spoon: All without being soaked in solvent. Its area is twice the sum of the area of ​​1 ellipse plus the area of ​​2 trapezoids plus the area of ​​1 trapezoid. The calculation formula is shown in formula (2).
(2×(×h)
+[(E+F)×h
[(E+F)Xh2
0. 785 × Dd +(A +B) ×h +
The meaning of each letter in formula (2) is shown in Figure 1.
A——The length of the upper semicircle of the spoon:
B—The length of the lower semicircle of the spoon.
4.4.2 Chopsticks (square tail and round head): All immersed in the solvent. Its area is the sum of the area of ​​the rectangle and the area of ​​the cylinder. S=A2+4Ah,+Dh
The meaning of each letter in formula (3) is shown in Figure 2.
4.4.3 Bottle cap: All immersed. Its area is twice the sum of the area of ​​the ring and the area of ​​the circumference. S=2[(-r)+2mh]
The meaning of each letter in formula (4) is shown in Figure 3.
（2）
（3）
4.4.4 Bowl edge: For those with floral decorations on the edge, put them in the solvent and immerse them 2cm deep. Its area is twice the area of ​​the side of the immersed cone. times. S=[yuanl(n+r)]x2=4yuan(+r2)
For the meaning of each letter in formula (5), see Figure 4.
GB/T5009.156-2003
4.4.5 Edge of cylindrical cup mouth: Those with floral decorations on the edge are turned upside down in the solvent and immersed 2cm deep. Its area is twice the area of ​​the cylinder without bubbles.
S=2yuan×2×2
=8yuanr
For the meaning of each letter in formula (6), see Figure 5.
4.4.6 Soup spoon: Its area is the area of ​​the spherical crown. S=(r+h)
When fully immersed, multiply by 2.
For the meaning of each letter in formula (7), see Figure 6.
4.4.7 Plastic beverage straw: fully immersed. Its area is twice the measured area of ​​the cylinder. S= Dh ×2
The meaning of each letter in formula (8) is shown in Figure 7.
Note: In the above formulas, S refers to the area, D
5The cleaning of the sample
diameter-radius.
The sample is rinsed with tap water and then cleaned with dishwashing detergent (GB9985). After repeated rinsing with tap water, it is rinsed with distilled water or deionized water for 2 to 3 times and dried in an oven. Products such as plastics and rubber that are not suitable for baking should be dried. If necessary, the surface moisture of the product can be absorbed with clean filter paper, but paper fibers must not remain on the surface of the appliance. The cleaned sample should be protected from dust contamination, and the cleaned surface should not be touched directly by hand. || tt||6 Preparation of soaking solution
6.1 Solvent
Select the solvent (water, 4% acetic acid, ethanol and n-hexane) of simulated food according to the purpose of the test. The percentage concentration of solvent refers to the volume fraction. 6.2 Soaking method
6.2.1 Hollow products
Accurately measure the solvent according to the sample volume measured by the above method and add it to the hollow product, and soak it according to the test conditions (temperature, time) specified for the product. Plastic containers larger than 1.1L can also be cut into test pieces for measurement. Plastic film bags that can hold solvents should soak the inner wall without text and patterns. The bag mouth can be opened and placed in a beaker of appropriate size, and an appropriate amount of solvent is added for soaking according to the law. Composite food packaging bags are calculated at 2mL per square centimeter 307
GB/T5009.156-—2003bzxz.net
m, and the solvent is injected and soaked according to the law.
6.2.2 After measuring the area of ​​the flat product, inject the specified solvent at a volume of 2mL per square centimeter and soak it in accordance with the law. Or the method of soaking all the way can be used, and the area should be calculated on two sides. 6.2.3 Plates, films and test pieces are soaked in the same way as flat products. 6.2.4 For rubber products, add 2 mL of soaking liquid per square centimeter of contact area. If the contact area cannot be calculated, add 20 mL of soaking liquid per gram of sample.
6.2.5 For drip plastic gaskets that can be peeled off in one piece, add 2 mL of soaking liquid per square centimeter. For those that cannot be peeled off in one piece, cut the thicker part of the edge into strips with a width of 0.3 cm to 0.5 cm and a length of 1.5 cm to 2.5 cm, and weigh them. Add 60 mL of soaking liquid per gram of sample. 6.3 Precautions
6.3.1 The total amount of soaking liquid should be able to meet the needs of each measurement item. For example, in most cases, each soaking liquid for the determination of evaporation residue should be no less than 200 mL, and each soaking liquid for the determination of potassium permanganate consumption should be no less than 100 mL. 6.3.2 When soaking with 4% acetic acid, the required amount of water should be heated to the required temperature first, and then the calculated amount of 36% acetic acid should be added to make its concentration reach 4%.
6.3.3 During the soaking, the sample should be carefully observed and stirred appropriately when necessary, and any bubbles that may be attached to the sample surface should be removed. 6.3.4 After the soaking, the solvent should be observed for evaporation loss, otherwise fresh solvent should be added to make up to the original volume. 6.3.5 See Appendix B for soaking conditions.
7 Calculation of results
7.1 Hollow products: It can be expressed in grams per liter (mg/L). 7.2 Flat products
7.2.1 If the amount of soaking solution used is exactly 2mL per square centimeter, the measured value is the amount of sample migration precipitation (mg/L). 7.2.2 If the amount of immersion liquid used is more or less than 2 mL per square centimeter, the measured value (mg/L) shall be used to calculate according to formula (9): ao
Wherein:
Migrant precipitate, unit is milligram per liter (mg/L); - measured value, unit is milligram per liter (mg/L); V - immersion liquid volume, unit is milliliter (mL); S - flat product reference area, unit is square centimeter (cm\); 2 - number of milliliters of solvent required per square centimeter of area. 7.2.3 When the amount of precipitate of the flat product sample is expressed in mg/dm2, it shall be calculated according to formula (10): ao=
Wherein:
Migrant precipitate, unit is milligram per square decimeter (mg/dm\); c - measured value, unit is milligram per liter (mg/L); V - immersion liquid volume, unit is liter (L); A - sample reference area, unit is square decimeter (dm2). (9)
(10)
Note: When this formula is used, the unit of length measured in the reference area measurement item of 4.2 for flat products is expressed in decimeters (dm) (1dm10cm), and the unit of area is expressed in square decimeters (dm2) (1dm2=100cm). 7.3 The calculation method for sheets, films, composite food packaging bags and test pieces is the same as that for flat products, but the area is the actual measured area. 308
Plastic resin
Plastic moldings and
Composite food packaging bags
Plastic film bags
Plastic film
Aluminum products, porcelain
Ceramic products
Stainless steel products
(including rubber tubes)
Base paper for food packaging
Rubber nipples
Rubber products for food
Appendix A
(Normative Appendix)
Sampling method for food packaging materials
Sampling method
GB/T5009.156—2003
Randomly select 10% of the number of packages, and the small batch shall not be less than 3 packages. Randomly take 2kg of each package and mix it. Use the quartering method to reduce it to 500g for a total of three parts. Randomly sample 0.1% of the output. The small batch is not less than 10 pieces. Take 20 pieces of less than 500mL capacity. Randomly take 10 bundles from each batch. Cut a 50cm×50cm piece from each bundle, a total of 10 pieces. Cut it into 5cm×5cm samples for inspection and mix it thoroughly. Randomly sample 0.1% of the output for products with the same shape, size, and flower decoration. Take 10 pieces of less than 500mL capacity for a small batch of not less than 6 pieces. Focus on extracting utensils with strong colors or small area-to-volume ratios. Randomly cut five pipes of the same material and inner diameter with appropriate lengths so that their capacity can meet the needs of the measurement. The length is calculated as follows: In the formula:
Tube length #
—Required number of milliliters of soaking liquid:
One tube inner diameter.
Note: The actual length of the cut tube should be L + a, where α is the length of the area occupied by the glass plugs at both ends. The manufacturer shall prepare 6 to 10 pieces of metal sheets with a thickness of less than 2mm and a full coating test piece of 10cm×10cm or 5cm×15cm for inspection under the same process conditions of the product. If the test piece provided is a single-sided coating, the substrate shall be provided as a control. Randomly sample 500g from each batch, and randomly cut 10 pieces of 10cm×10cm. Randomly sample 500g from each batch. Randomly sample 500g from each batch. There shall be no less than 6 pressure cooker sealing rings in each batch. 309
GB/T5009.156—2003
B.1 Plastic products
Plastic products shall comply with the provisions of Table B.1.
Polyethylene (PE), polystyrene (PS), polypropylene (PP), trimerized amine (MA), unsaturated polyester and fiberglass products, foamed polytetrafluoroethylene (PTFE)
polyvinyl chloride (PVC)
nylon 6 (PA)
polyethylene terephthalate (PET)
resin·
Appendix B
(Normative Appendix)
Foaming test items and test conditions
Inspection items||t t||n-Hexane Extract
Potassium Permanganate Consumption
Evaporation Residue
Molding Product
Heavy Metal
Formaldehyde?
Bottle Pad Granules
Molding Product
Resin Molding Product
Molding Product
Potassium Permanganate Consumption Pan
Evaporation Residue
Potassium Permanganate Consumption
Evaporation Residue
Heavy Metal
Caprolactam
Lead (Pb)
Sb
Extract||tt ||Potassium permanganate consumption plate
Evaporation residue
Heavy gold phoenix
Antimony (Sb)
N-hexane
4% acetic acid
65% ethanol
N-hexane
4% acetic acid
4% acetic acid
4% acetic acid
4% acetic acid
20% ethanol
N-hexane
4% acetic acid
4% acetic acid
4% acetic acid
4% acetic acid
65% ethanol
N-hexane Alkane
4% acetic acid
65% ethanol
n-hexane
4% acetic acid
4% acetic acid
Test conditions
Room temperature (>20℃)
Room temperature (>20℃)
Room temperature (>20℃)
100℃
Room temperature (>20℃)
Room temperature (>20℃)
Resin and molded products
Polycarbonate (PC)
Composite food packaging bags
Refers to PE, PS, and PP resins.
Table B.1 (continued)
Inspection items
Extract
Heavy metals
Potassium manganate consumption
Evaporation residue
Heavy metals
Diaminotoluene
4% acetic acid
20% ethanol
n-hexane
4% acetic acid
4% acetic acid
65% ethanol
n-hexane
4% acetic acid
PP does not measure 65% ethanol residue, PS does not measure n-hexane residue, MA only measures water evaporation residue. Refers to MA.
GB/T5009.156—2003
Test conditions
Room temperature (>20℃)
Room temperature (>20℃)
100℃
Including PVC bottle cap gaskets. The finished product is added with water soaking liquid (60℃, 0.5h) to measure the evaporation residual flow, and the bottle cap gaskets that contact high-ethanol food are added with 65% ethanol evaporation residue.
No bubble temperature: Resin slightly boiling reflux; molding product normal hexane room temperature (>20℃), others 95℃±5℃. e
B.2 Gold-extension products
Gold-extension products should comply with Table B.2.
Aluminum products
Cookers
Stainless steel products
Inspection items
Zinc (Zn)
Lead (Pb)
Pot (Cd)
Arsenic (As)
Lead (Pb)
Arsenic (As)
Chromium (Ct)
Nickel (Ni)
Test conditions
4% acetic acid
4% acetic acid
Room temperature (>20℃)
Boiling for 0.5h
Boiling for 0.5h
Leaving for 24h
Leaving for 24h
GB/T5009.156-2003
Sugar porcelain products
a refers to leaving at room temperature for 24h.
Ceramic products
Ceramic products shall comply with the provisions of Table B.3.
Ceramic products
a refers to 24 hours at room temperature.
Paint samples and base paper
Test items
Lead (Pb)
Cd
Table B.2 (continued)
Test items
Lead (Pb)
Cd
Antimony (Sb)
Paint samples and base paper shall comply with the provisions of Table B.4. Name
Epoxy phenolic resin for inner wall of can
Resin, coating, coating film; demoulding
Coating film; water-based modified epoxy
epoxy can inner wall coating
Perchlorethylene coating
Inspection items
Consumption of potassium permanganate
Evaporation residue
Heavy metal
Free phenol
Free formaldehyde
Consumption of potassium permanganate
Evaporation residue
Lead (Pb)
Arsenic (As)
4% acetic acid
4% acetic acid| |tt||20% ethanol
n-hexane
4% acetic acid
4% acetic acid
65% ethanol
4% acetic acid
4% acetic acid
4% acetic acid
Test conditions
Test conditions
Test conditions
Leave for 24ha
Leave for 24h
Urushiol coating
Silicone anti-stick coating film
Polytetrafluoroethylene coating film
Polyamide cyclopentane in container
Oxygen resin coating||tt ||Base paper for food packaging
Inspection items
Consumption of potassium permanganate
Evaporation residue
Heavy metals
Free phenol
Consumption of potassium permanganate
Evaporation residue
Heavy metals
Consumption of potassium permanganate
Evaporation residue
Chromium (Cr)）
Fluorine (F)
Consumption of potassium permanganate
Evaporation residue
Heavy metals
Lead (Pb), arsenic (As)
Fluorescence inspection||tt ||Decolorization test
Table B.4 (continued)
4% acetic acid
65% ethanol
n-hexane
4% acetic acid
4% acetic acid
4% acetic acid
n-hexane
4% acetic acid
4% acetic acid
n-hexane
4% acetic acid
4% acetic acid
65% ethanol
n-hexane
4% acetic acid
Only free phenol is measured for epoxy phenolic resin and coating for inner wall of cans, and heavy metal phenol is not measured for coating film. n-hexane residue is not measured for water-based modified epoxy coating for inner wall of cans. Refers to being placed at room temperature for 24 hours.
B.5 Rubber products
Rubber products shall comply with the provisions of Table B.5.
Test conditions
Room temperature (>20℃)
Room temperature (>20℃)
Boiling for 0.5h
Boiling for 0.5h
Boiling for 0.5h
Room temperature (>20℃)
Boiling for 0.5h
Boiling for 0.5h
Room temperature (>20℃)
GB/T5009.156—2003
Leave for 24h2
Leave for 24h2s
Leave for 24h3
Leave for 24h)
Soak in water and n-hexane to observe the color156—2003
Leave for 24h2
Leave for 24h
Leave for 24h2s
Leave for 24h3
Leave for 24h)
Soak in water and n-hexane to observe the color156—2003
Leave for 24h2
Leave for 24h
Leave for 24h2s
Leave for 24h3
Leave for 24h)
Soak in water and n-hexane to observe the color
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