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食品安全国家标准 食品接触材料及制品迁移试验预处理方法通则
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GB 5009.156-2016
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标准编号: GB 5009.156-2016 (GB5009.156-2016)
中文名称: 食品安全国家标准 食品接触材料及制品迁移试验预处理方法通则
英文名称: General principle for the determination of migration of packaging materials and their products
行业: 国家标准
中标分类: X09
字数估计: 20,233
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 5009.156-2003
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 5009.156-2016: 食品安全国家标准 食品接触材料及制品迁移试验预处理方法通则
GB 5009.156-2016 英文名称: General principle for the determination of migration of packaging materials and their products
中 华 人 民 共 和 国 国 家 标 准
GB5009.156—2016
食品安全国家标准
食品接触材料及制品迁移
试验预处理方法通则
中华人民共中和国国家卫生和计划 生育 委员会 发 布
1 范围
本标准规定了食品接触材料及制品迁移试验预处理方法的试验总则、试剂和材料、设备与器具、采样与制样方法、
试样接触面积、试样接触面积与食品模拟物体积比、试样的清洗和特殊处理、试验方法、 迁移量的测定要求和结果表述要求。
本标准适用于食品接触材料及制品的迁移试验预处理。
2 术语和定义
3 试验总则
3.1 本标准为食品接触材料及制品迁移试验预处理方法，经预处理获得的浸泡液应按照相关检验方法标准的规定进行迁移量测定。相应食品安全国家标准对于迁移试验预处理有特殊规定时，应符合相应 标准的规定。
3.2 食品接触材料及制品迁移试验条件及食品模拟物的选择应按照GB31604.1及相关产品标准的规
定执行。
3.3 迁移试验测定对象为在合理预期使用条件下可能与食品直接接触的面。
4 试剂和材料
除非另有说明，本方法所用试剂均为分析纯，水为 GB/T 6682规定的一级水。
4.1 试剂
4.2 试剂配制
4.2.1 4%乙酸溶液(体积分数):量取20.0 mL 冰乙酸(4.1.1),加480 mL 水，混匀。
4.2.2 10%乙醇溶液(体积分数):量取50.0 mL 无水乙醇(4.1.2),加450 mL 水，混匀。
4.2.3 20%乙醇溶液(体积分数):量取100.0 mL 无水乙醇(4.1.2),加400 mL 水，混匀。
4.2.4 50%乙醇溶液(体积分数):量取250.0 mL 无水乙醇(4.1.2),加250 mL 水，混匀。
4.2.5 65%乙醇溶液(体积分数):量取325.0 mL 无水乙醇(4.1.2),加175 mL 水，混匀。
4.2.6 0.1mol/L 硝酸溶液：量取6.4 mL 硝酸(4.1.9)加入水中，并定容至1000 mL。
4.2.7 0.1mol/L 氢氧化钠溶液：称取1.0 g 氢氧化钠(4.1.8)于聚乙烯或聚四氟乙烯塑料烧杯中，加水溶解至250 mL。 冷却后，转移到塑料(PET 除外)瓶中，待用。
5 设备与器具
5.1 天平
感量为1 mg。
5.2 试样支架
试样支架应能够支撑试样，保持试样之间分开，且保证试样与模拟物完全接触，其材质不影响迁移量测定结果。支架的选择参见附录B 中图B.1、图 B.2,也可使用其他符合要求的支架。
5.3 玻璃棒和玻璃珠
用于对食品模拟物的液位进行细微调整，以使试样表面完全浸入模拟物中，也可采用其他合适 方法。
5.4 迁移测试池
迁移测试池应无渗漏，其材质不影响迁移量测试结果。挥发性物质的测定应使用气密性的迁移测试池和顶部预留空间较小的迁移测试池。迁移测试池的种类参见附录B 中图 B.3～图 B.6,也可使用其 他符合要求的迁移测试池。
5.5 恒温设备
恒温设备(恒温箱、培养箱、水浴锅、冰箱等)应保证迁移试验达到规定的温度，并可控制食品模拟物 温度，温度的误差应符合附录C 中表 C.1 的规定。
6 采样与制样方法
6.1 所采样品应具有代表性。样品应完整、无变形、规格一致。采样数量应能满足检验项目对试样量的需要，供检测与复测之用。
6.2 样品的采集和存储应避免样品受污染和变质。当试样含有挥发性物质时，应采用低温保存或密闭保存等方式。
6.3 迁移试验预处理应尽可能在样品原状态下进行。如因技术原因无法对样品进行直接测试，可将样品进行切割或按照实际加工条件制得符合测试要求的试样。切割时，应避免对试样测试表面造成机械 损伤，应尽可能将切割操作过程产生的试样温升降至最低。
6.4 对于组合材料及制品，应尽可能按接触食品的各材质材料的要求分别采样。
6.5 对于形状不规则、容积较大或难以测量计算表面积的制品，可采用其原材料(如板材)或取同批制 品中有代表性制品裁剪一定面积板块作为试样。
6.6 对于树脂或粒料、涂料、油墨和粘合剂等与实际成型品有明显差异的食品接触材料，应当按照实际 加工条件制成成型品或片材进行迁移试验预处理。
7 试样接触面积
7.1 一般要求
应采用合适的方法准确测定试样中与食品模拟物接触的面积。不同形态试样面积的测定参照 7.2～7.6进行，也可采用其他准确测定面积的方法。
7.2 空心制品面积
空心制品的面积为接触食品模拟物的面积总和，即接触食品模拟物的空心制品的内底部和内侧面 面积之和。有规格的空心制品按其规格计算；无规格的空心制品，食品模拟物液面与空心制品上边缘 (溢出面)的距离不超过1 cm。需加热煮沸的空心制品加入食品模拟物的量应能保证加热煮沸时液体
不会溢出，接触容积不得小于容积的4/5。边缘有花彩者应浸过花面。
7.3 扁平制品面积
将扁平制品(一体的圆形口)反扣于纸上，沿制品边缘画下轮廓，记下此参考面积(S) 。对于圆形的扁平制品可以量取其直径(D) 按式(1)计算其参考面积。对于盛放食品模拟物时液面至上边缘的距离
小于1cm 的扁平制品，将制品反扣于纸上，沿制品边缘画下轮廓，轮廓面积即为制品单面面积。
7.4 全浸没法中试样面积
全浸没试验时，试样厚度小于或等于0.5 mm 时，计算面积取试样的单面面积；试样厚度大于 0.5 mm并且小于或等于2 mm 时，计算面积取试样正反两面面积之和，即单面面积乘以2;试样厚度大 于 2 mm 时，计算面积取试样正反两面面积及其侧面积之和。
7.5 迁移测试池法中试样面积
试样面积以试样实际接触食品模拟物或其他化学溶剂的面积计算。
7.6 不同形状的制品面积测定方法举例
7.2～7.5未包含的部分特殊形状的制品面积测定方法实例参见附录D。
8 试样接触面积与食品模拟物体积比(S/V)
8.1 采用不同的试验方法，选择合适的 S/V 对试样进行迁移试验预处理。
8.2 因技术原因无法采用实际的 S/V 或常规 S/V(6dm²接触面积对应1L 或1kg 食品模拟物)时， 可调整 S/V使模拟物中待测迁移物达到合适的浓度以满足方法检测要求。
8.3 迁移试验预处理中试样 S/V 应确保在整个试验过程中，食品模拟物中待测迁移物的浓度始终处 于不饱和状态。
9 试样的清洗和特殊处理
9.1 试样应洁净，无污染。
9.2 试样应按实际使用情形进行清洁。使用前无需清洗的试样(如一次性餐具)可用不脱绒毛布或软 刷清除试样表面的异物。
9.3 使用前有清洗或特殊处理要求的试样，按照标签或说明书上的要求进行清洗或处理后，用蒸馏水 或去离子水冲2次～3次，自然晾干，必要时可用洁净的滤纸将试样表面水分吸干净，但纸纤维不得存 留试样表面。
9.4 清洗或处理过的试样应防止污染，且不得用手直接接触试样表面，应用镊子夹持或戴棉质手套传递试样。
10 试验方法
10.1 一般要求
10.1.1 迁移试验预处理过程中，如食品模拟物受热蒸发导致体积减少，应加入食品模拟物定容至原 体积。
10.1.2 测定挥发性物质时，应采用适宜的密封措施以防止待测物质损失。
10.1.3 迁移试验时间应从食品模拟物达到选定的迁移试验温度后开始计时，迁移试验时间的误差应符合附录C中表C.2的规定。
10.1.4 迁移试验预处理结束后，应将浸泡液立即转移至干净的器皿中以备后续迁移量测定使用。
10.1.5 进行迁移试验预处理时，应同时做空白试验。
10.2 灌装法
10.2.1 一般方法
10.2.2 制袋法
塑料膜(袋)、复合包装膜(袋)等也可采用制袋法，封合好后切开袋子的一角，其孔径便于注入食品 模拟物，将试样袋放入试样支架(如图 B.2所示的支架或类似装置)中。将已达到试验温度的食品模拟 物注入试样袋中，开口角热封或用夹子固定。
GB 5009.156-2016
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
National food safety standard
General principle of migration test pre-treatment
method of food contact materials and their products
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of contents
Foreword ... 3
1 Scope ... 4
2 Terms and definitions ... 4
3 General principles of test ... 4
4 Reagents and materials ... 5
5 Equipment and instruments ... 7
6 Sampling and sample preparation method ... 8
7 Sample contact area ... 8
8 Ratio between sample contact area and food simulant volume (S/V) ... 10
9 Sample cleaning and special treatment ... 10
10 Test methods ... 11
11 Determination requirements of migration quantity ... 13
12 Results presentation requirements ... 13
Appendix A Requirements for fatty food simulant ... 15
Appendix B Holder and migration test basin ... 16
Appendix C Migration test temperature and time error ... 21
Appendix D Examples of determination methods for the area of special shape
products ... 22
Foreword
This standard replaces GB/T 5009.156-2003 “General principles of soaking
test method of food packaging materials and their products”.
As compared with GB/T 5009.156-2003, the main changes of this standard are
as follows.
- CHANGE the standard name into “National food safety standard - General
principle of migration test pre-treatment method of food contact materials
and their products”;
- MODIFY the terms and definitions;
- ADD the general principles of test;
- ADD the reagents and materials;
- ADD the equipment and instrument;
- MODIFY the sampling and sample preparation methods;
- MODIFY the sample contact area;
- ADD the ration between sample contact area and food simulant volume;
- MODIFY the sample cleaning;
- MODIFY the test method;
- ADD the determination requirements for migration quantity;
- MODIFY the result presentation requirements;
- DELETE the “Appendix A. Sampling method of food packaging materials”
from the original standard;
- DELETE the “Appendix B. Soaking test items and test conditions” from the
original standard;
- ADD the Appendix A, Appendix B, Appendix C, and Appendix D.
National food safety standard
General principle of migration test pre-treatment
method of food contact materials and their products
1 Scope
This standard specifies the general principles of test, reagents and materials,
equipment and instruments, sampling method and sample preparation
methods, sample contact area, ratio between sample contact area and food
simulant volume, sample cleaning and special treatment, test method,
determination requirements of migration quantity, and result presentation
requirements of the migration test pre-treatment method of food contact
materials and their products.
This standard applies to the migration test pre-treatment method of food
contact materials and their products.
2 Terms and definitions
2.1 Migration test basin
It refers to the device used to install and fix the sample to be tested, and
conduct the migration test pre-treatment after injecting the food simulant.
It refers to the products for which the depth from the product mouth along the
horizontal plane to its internal lowest horizontal plane is more than 25 mm.
2.3 Flat products
It refers to the products for which the depth from the product mouth along the
horizontal plane to its internal lowest horizontal plane is less than or equal to
25 mm.
3 General principles of test
3.1 This standard provides the migration test pre-treatment method of food
contact materials and their products. The soaking solution as obtained through
mg/L; HCO3-, 44.0 mg/L; Cl-, 28.4 mg/L; SO42-, 13.0 mg/L; Na+, 16.0 mg/L.
STORE it in a closed container; AND the shelf life shall be not more than 7 d.
4.2.12 0.1 mol/L hydrochloric acid solution. TAKE 9 mL of hydrochloric acid
(4.1.17); ADD it into water and MAKE its volume reach to 1000 mL.
4.2.13 Artificial saliva. DISSOLVE 4.2 g of sodium bicarbonate (4.1.10), 0.5 g
of sodium chloride (4.1.14), 0.2 g of potassium carbonate (4.1.15) and 30 mg
of sodium nitrite (4.1.16) into water; DILUTE it to 900 mL. ADJUST the pH to
9.0. If necessary, ADD 0.1 mol/L hydrochloric acid solution (4.2.12) or 0.1
mol/L sodium hydroxide solution (4.2.7). TRANSFER it to a 1000 mL
5 Equipment and instruments
5.1 Balance
The sensitivity is 1 mg.
5.2 Sample holder
The sample holder shall be capable of supporting the sample, maintaining the
separation between the samples, and ensuring that the sample is in complete
contact with the simulant, AND its material shall be such as not affect the
determination results of the migration quantity. As for the holder selection, SEE
Figure B.1 and Figure B.2 in Appendix B; AND it may also use other holders
5.3 Glass rod and glass bead
It is used to fine-tune the liquid level of the food simulant so that the surface of
the sample is completely immersed in the simulant; AND it may also use other
appropriate methods.
5.4 Migration test basin
The migration test basin shall be free of leakage AND its material shall not
affect the migration test results. The determination of volatile substances shall
be carried out using a gas-tight migration test basin and a migration test basin
with a smaller reserved space at the top. As for the types of the migration test
migration test basins complying with requirements.
5.5 Constant temperature equipment
In case of full immersion test, when the sample thickness less than or equal to
0.5 mm, the calculated area takes the single-sided area of the sample; when
the sample thickness is more than 0.5 mm and less than or equal to 2 mm, the
calculated area takes the sum of the positive side area and the negative side
area, that is, the single-sided area multiplied by 2; when the sample thickness
is greater than 2 mm, the calculated area takes the sum of the positive side
area, the negative side area, and the side area.
The sample area is calculated as the area of the sample which is actually in
contact with the food simulant or other chemical solvents.
7.6 Examples of methods for determining the area of products of
different shapes
As for the examples of the determination methods on the area of products of
some special shapes not covered in 7.2 ~ 7.5, SEE Appendix D.
8 Ratio between sample contact area and food
simulant volume (S/V)
8.1 USE different test methods and SELECT appropriate S/V to conduct the
8.2 When the actual S/V or conventional S/V (6dm2 contact area corresponds
to 1 L or 1 kg of food simulant) cannot be used for technical reasons, it may
adjust the S/V to make the migration substance to be tested in the simulant
reach to appropriate concentration, in order to satisfy the method testing
requirements.
8.3 The sample S/V in the migration test pre-treatment shall ensure that in the
entire test process, the concentration of the migration substances to be tested
in the food simulant is always in an unsaturated state.
9 Sample cleaning and special treatment
9.2 Samples shall be cleaned in accordance with the actual conditions of use.
As for the samples which do not need cleaning before use (such as disposable
constant temperature equipment which had reached to the test temperature,
and CONDUCT the migration test in accordance with specified test conditions
(temperature and time). As for the samples of the plastic film bags and
composite bags and others, it shall use the surface expected to be in contact
with the food as the test surface, place the bag into the beaker of appropriate
size, add appropriate amount of food simulant which had reached to the test
temperature into the bag, to make it contact with the region the area of which
accordance with the test conditions as specified for this sample.
10.2.2 Bagging method
Plastic films (bags) and composite packaging film (bags) may also use the
bagging method. After sealing it, CUT one corner of the bag, to make an
aperture of such size as able to accommodate the injection of the food
simulant; PLACE the sample bag into the sample holder (the holder as s...
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