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食品安全国家标准 食品接触材料及制品 氯乙烯的测定和迁移量的测定
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GB 31604.31-2016
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标准编号: GB 31604.31-2016 (GB31604.31-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 氯乙烯的测定和迁移量的测定
英文名称: Determination of residual ethylidene dichloride in polyvinyl chloride resin and product for food container and packaging material
行业: 国家标准
中标分类: X09
字数估计: 10,131
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2898-2011; GB/T 5009.68-2003部分; GB/T 5009.67-2003; GB/T 5009.122-2003; GB/T 23296.14-2009; GB/T 23296.13-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.31-2016: 食品安全国家标准 食品接触材料及制品 氯乙烯的测定和迁移量的测定
GB 31604.31-2016 英文名称: Determination of residual ethylidene dichloride in polyvinyl chloride resin and product for food container and packaging material
1 范围
本标准规定了食品接触材料用塑料及其制品中氯乙烯的测定和氯乙烯迁移量的测定方法。
本标准适用于聚氯乙烯或氯乙烯共聚物中氯乙烯的测定和迁移量的测定。
本标准也适用于聚氯乙烯或聚氯乙烯共聚物中1,1-二氯乙烷的测定。
2 原理
将试样放入密封平衡瓶中,用N,N-二甲基乙酰胺溶解。在一定温度下,氯乙烯扩散,当达到气液
平衡时,取液上气体注入气相色谱仪,氢火焰离子化检测器测定,外标法定量。
3 试剂与材料
除非另有说明,所有试剂均为分析纯。
3.1 试剂
N,N-二甲基乙酰胺:纯度大于99%。
3.2 标准品
氯乙烯基准溶液:5000mg/L,丙酮或甲醇作溶剂。
3.3 标准溶液配制
3.3.1 氯乙烯储备液的配制(10mg/L):在10mL棕色玻璃瓶中加入10mLN,N-二甲基乙酰胺,用
微量注射器吸取20μL氯乙烯基准溶液到玻璃瓶中,立即用瓶盖密封,平衡2h后,保存在4℃冰箱中。
3.3.2 氯乙烯标准工作溶液的配制:在7个顶空瓶中分别加入10mLN,N-二甲基乙酰胺,用微量注射
器分别吸取0μL、50μL、75μL、100μL、125μL、150μL、200μL氯乙烯储备液缓慢注射到顶空瓶中,
立即加盖密封,混合均匀,得到 N,N-二甲基乙酰胺中氯乙烯浓度分别为0mg/L、0.050mg/L、
0.075mg/L、0.100mg/L、0.125mg/L、0.150mg/L、0.200mg/L。
4 仪器与设备
4.1 气相色谱仪:配置自动顶空进样器和氢火焰离子化检测器。
4.2 玻璃瓶:10mL,瓶盖带硅橡胶或者丁基橡胶密封垫。
4.3 顶空瓶:20mL,瓶盖带硅橡胶或者丁基橡胶密封垫。
4.4 微量注射器:25μL、100μL、200μL。
4.5 分析天平:感量0.0001g和0.01g。
5 分析步骤
5.1 试液制备
称取1g(精确到0.01g)剪碎后的试样(面积不大于1cm×1cm)于顶空瓶中,加入10mL的N,N-二
甲基乙酰胺,立即加盖密封,振荡溶解(如果溶解困难,可适当升温),待完全溶解后放入自动顶空进样器
待测。
5.2 测定
5.2.1 仪器参考条件
5.2.1.1 自动顶空进样器条件
a) 定量环:1mL或3mL;
b) 平衡温度:70℃;
c) 定量环温度:90℃;
d) 传输线温度:120℃;
e) 平衡时间:30min;
f) 加压时间:0.20min;
g) 定量环填充时间:0.10min。
注:如采用手动顶空进样,参考方法见附录A。
5.2.1.2 色谱条件
a) 色谱柱:聚乙二醇毛细管色谱柱,长30m,内径0.32mm,膜厚1μm,或等效柱;
b) 柱温程序:起始40℃,保持1min,以2℃/min的速率升至60℃,保持1min,以20℃速率升
至200℃,保持1min;
c) 载气:氮气,流速1mL/min;
d) 进样模式:分流,分流比1∶1;
e) 进样口温度:200℃;
f) 检测器温度:200℃。
5.2.2 标准工作曲线的制作
对3.3.2中制备的标准工作溶液在5.2所列仪器参数下进行检测,以氯乙烯标准工作溶液质量浓度
为横坐标,以对应的峰面积为纵坐标,绘制标准工作曲线,得到线性方程。标准溶液色谱图见附录B。
5.2.3 定量测定
对5.1中制备的样品在5.2所列仪器参数下进行检测,根据氯乙烯色谱峰峰面积,由标准曲线计算
出样液中氯乙烯单体量。
6 分析结果的表述
结果保留两位有效数字。
7 精密度
在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的10%。
8 其他
本标准中氯乙烯的检出限0.1mg/kg,定量限为0.5mg/kg。
氯乙烯迁移量的测定
9 原理
将食品模拟物放入密封平衡瓶中,在一定温度下,氯乙烯扩散,当达到气液平衡时,取液上气体注入
气相色谱仪,氢火焰离子化检测器测定,外标法定量。
10 试剂与材料
除非另有说明,所有试剂均为分析纯。
10.1 试剂
10.1.1 水性、酸性、酒精类、油脂类食品模拟物:按GB 31604.1的规定。
10.1.2 N,N-二甲基乙酰胺:纯度大于99%。
10.2 试剂配制
水性、酸性、酒精类、油脂类食品模拟物:按GB 5009.156配制。
10.3 标准品
氯乙烯基准溶液:5000mg/L,丙酮或甲醇作溶剂。
10.4 标准溶液配制
10.4.1 氯乙烯储备液:在6个10mL玻璃瓶中分别加入10mLN,N-二甲基乙酰胺,在每个瓶中依次
加入5μL、10μL、20μL、30μL、40μL、50μL氯乙烯基准溶液,立即密封玻璃瓶,混合均匀,得到氯乙烯
10.4.2 水性食品模拟物标准工作溶液:在6个顶空瓶中分别加入10mL水,向每个顶空瓶中依次加入
不同浓度的氯乙烯储备液20μL,立即加盖密封,混合均匀,得到水中氯乙烯浓度依次为0.0050mg/L、
0.010mg/L、0.020mg/L、0.030mg/L、0.040mg/L和0.050mg/L。采用同样方式,分别用酸性、酒精
类食品模拟物配制同样浓度系列的氯乙烯标准工作溶液。
10.4.3 油脂类食品模拟物标准工作溶液:分别称取10g(精确至0.1g)油脂类食品模拟物于6个顶空
瓶中,向每个顶空瓶中依次加入不同浓度的氯乙烯储备液20μL,立即加盖密封,混合均匀,得到油脂类
食品模拟物中氯乙烯浓度依次为0.0050mg/kg、0.010mg/kg、0.020mg/kg、.030mg/kg、.040mg/kg和0.050mg/kg。
注:标准溶液配制前,食品模拟物需提前在4℃冰箱中充分冷却,标准溶液配制过程中操作应快速。
11 仪器与设备
11.2 分析天平:感量0.0001g,0.01g。
11.3 玻璃瓶:10mL,瓶盖带硅橡胶或者丁基橡胶密封垫。
11.4 顶空瓶:20mL,瓶盖带硅橡胶或者丁基橡胶密封垫。
11.5 微量注射器:10μL、25μL、50μL。
12 分析步骤
12.1 食品模拟物试液的制备
12.1.1 总则
本标准食品模拟试验采用水性、酸性、酒精类、油脂类食品模拟物,可以包括水性食品、酸性食品、含酒精类饮料和脂肪类食品。所需试液通过迁移试验获取,可在4℃冰箱中避光保存1周。
GB 31604.31-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the
Vinyl Chloride and Determination of Migration
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Apparatus ... 5
5 Analytical procedures ... 5
6 Expression of Analytical Results ... 7
7 Precision ... 7
8 Others ... 7
9 Principle ... 7
10 Reagents and Materials ... 8
11 Apparatus ... 9
12 Analytical Procedures ... 9
13 Expression of Analytical Results ... 10
14 Precision ... 10
15 Others ... 10
Appendix A Manual Sample Injecting Method ... 11
Appendix B Vinyl Chloride Standard Solution Gas Chromatogram ... 12
National Food Safety Standard – Food Contact
Materials and Articles – Determination of the Vinyl
Chloride and Determination of Migration
1 Scope
This Standard specifies the determination of the vinyl chloride and determination of
migration in plastic and products for food contact materials.
This Standard is applicable to the determination of vinyl chloride and determination of
migration in polyvinyl chloride and vinyl chloride copolymers.
This Standard is also applicable to the determination of 1,1-dichloroethane in polyvinyl
chloride and polyvinyl chloride copolymers.
Determination of Vinyl Chloride
2 Principle
Place the specimen into the sealed balance bottle; use N,N-Dimethylacetamide to
dissolve. At certain temperature, vinyl chloride is diffused; when the gas-liquid
equilibrium is reached, take gas above the liquid to inject into the gas chromatograph;
use hydrogen flame ionization detector to measure, use external standard method to
quantify.
3 Reagents and Materials
Unless otherwise is specified, all reagents shall be analytically pure.
3.1 Reagents
N,N-Dimethylacetamide. purity is greater than 99%.
3.2 Standard substance
Vinyl chloride reference solution. 5000mg/L; take acetone or methanol as solvent.
3.3 Preparation of standard solution
b) Equilibrium temperature. 70°C;
c) Quantitative loop temperature. 90°C;
d) Transmission line temperature. 120°C;
e) Balance time. 30min;
f) Pressurization time. 0.20min;
g) Filling time of quantitative loop. 0.10min;
h) Equilibration time of quantitative loop. 0.10min;
i) Sample injection time. 1.50min.
NOTE. if the manual headspace sampling injection is performed, the reference method can
refer to Appendix A.
5.2.1.2 Chromatographic conditions
a) Chromatographic column. polyethylene glycol capillary chromatographic column
with length of 30m, inner diameter of 0.32mm, film thickness of 1µm, or
equivalent column;
b) Column temperature program. maintain the initial temperature of 40°C for 1min;
raise the temperature to 60°C at the speed rate of 2°C/min, maintain for 1min;
raise the temperature to 200°C at the speed rate of 20°C [Translator note. here
c) Carrier gas. nitrogen, flow rate of 1mL/min;
d) Sample injecting mode. split, split ratio of 1.1;
e) Sample injecting temperature.200°C;
f) Detector temperature.200°C.
5.2.2 Drawing of standard working curve
The standard working solution prepared in 3.3.2 was tested under the instrumental
parameters listed in 5.2; take the mass concentration of vinyl chloride standard working
solution as abscissa; take the corresponding peak area as the ordinate; then draw the
standard working curve; obtain t he linear equation. Standard solution chromatogram
5.2.3 Quantitative determination
10 Reagents and Materials
Unless otherwise is specified, all reagents shall be analytically pure.
10.1 Reagents
10.1.1 Water-based, acidic, alcoholic, oil-fat food simulants. as per the provisions of
GB 31604.1.
10.1.2 N,N-Dimethylacetamide. purity greater than 99%.
10.2 Preparation of reagents
Water-based, acidic, alcoholic, oil-fat food simulants. prepare as per GB 5009.156.
Vinyl chloride reference solution. 5000mg/L; take acetone or methanol as solvents.
10.4 Preparation of standard solution
10.4.1 Vinyl chloride stock solution. separately add 10mL of N,N-Dimethylacetamide
into 6 pieces of 10mL glass bottles; successively add 5µL, 10µL, 20µL, 30µL, 40µL,
50µL of vinyl chloride into each bottle; mix evenly; then the concentrations of the
obtained vinyl chloride are 2.5mg/L, 5.0mg/L, 10.0mg/L, 15.0mg/L, 20.0mg/L,
25.0mg/L. Store into 4°C refrigerator.
10.4.2 Water-based food simulant standard working solution. separately add 10mL
of water into 6 headspace bottles; successively add 20mL of vinyl chloride stock
cap to seal; mix evenly; then the concentrations of the obtained vinyl chloride in water
are 0.0050mg/L, 0.010mg/L, 0.020mg/L, 0.030mg/L, 0.040mg/L and 0.050mg/L.
Adopting the same modes, separately use acidic, alcoholic food simulants to prepare
the vinyl chloride serial standard working solution with the same concentration.
10.4.3 Oil-fat food simulant standard working solution. respectively take 10g
(accurate to 0.1g) of oil-fat food simulants into 6 headspace bottles; successively add
20µ of vinyl chloride stock solution with different concentrations into each headspace
bottle; immediately use the cap to seal; mix evenly; the concentrations of the obtained
vinyl chloride in oil-fat food simulants are sequentially 0.0050mg/kg, 0.010mg/kg,
NOTE. before preparing the standard solution, food simulant needs to be fully cooled in the 4°C
refrigerator; the standard solution shall be prepared quickly.
12.3 Determination
12.3.1 Instrument reference condition
The same as 5.2.
12.3.2 Drawing of standard working curve
The standard working solution is tested as per the measurement conditions listed in
12.3.1. Take the concentration of vinyl chloride in the food simulant standard working
solution as the abscissa; while take the corresponding peak area as the ordinate; then
12.3.3 Quantitative determination
Sequentially inject the samples of food simulant test solution and blank test solution;
obtain the peak area of vinyl chloride chromatogram; deduct the blank value during the
calculating process. According to the peak area of vinyl chloride chromatogram,
calculate the concentration of vinyl chloride in sample solution by standard curve.
13 Expression of Analytical Results
The concentration of vinyl chloride in the sample solution is obtained from standard
curve; perform migration calculation as per GB 5009.156; obtain the migration of vinyl
chloride in the food contact materials and articles. The calculation results shall be
14 Precision
The absolute difference of two independent tests obtained under repeatability
conditions must not exceed 10% of the arithmetic mean.
15 Others
The detection limit of vinyl chloride in the water-based, acidic and alcoholic food
simulants is 0.001mg/L; quantitative limit is 0.005mg/L. The detection limit of vinyl
chloride in the oil-fat food simulant is 0.001mg/kg; quantitative limit is 0.005mg/kg.
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