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食品安全国家标准 食品接触材料及制品 锌迁移量的测定
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GB 31604.42-2016
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标准编号: GB 31604.42-2016 (GB31604.42-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 锌迁移量的测定
英文名称: Method for analysis of hygienic standard of rubber sheet (ring) for food use
行业: 国家标准
中标分类: X09
字数估计: 8,840
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2829-2011部分; GB/T 5009.79-2003部分; GB/T 5009.72-2003部分; GB/T 5009.66-2003部分; GB/T 5009.65-2003部分; GB/T 5009.64-2003部分
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.42-2016
Method for analysis of hygienic standard of rubber sheet (ring) for food use
中华人民共和国国家标准
食品安全国家标准
食品接触材料及制品 锌迁移量的测定
2016-10-19发布
2017-04-19实施
中 华 人 民 共 和 国
国家卫生和计划生育委员会 发 布
前言
本标准代替GB/T 5009.72-2003《铝制食具容器卫生标准的分析方法》、GB/T 5009.64-2003《食
品用橡胶垫片(圈)卫生标准的分析方法》、GB/T 5009.65-2003《食品用高压锅密封圈卫生标准的分析
方法》、GB/T 5009.66-2003《橡胶奶嘴卫生标准的分析方法》、GB/T 5009.79-2003《食品用橡胶管卫
生检验方法》和SN/T 2829-2011《食品接触材料 金属材料 食品模拟物中重金属含量的测定 电
感耦合等离子体发射光谱法》中锌迁移量的测定。
本标准与GB/T 5009.72-2003相比,主要变化如下:
---标准名称修改为“食品安全国家标准 食品接触材料及制品 锌迁移量的测定”;
---增加了火焰原子吸收光谱法;
---增加了电感耦合等离子体发射光谱法;
---增加了电感耦合等离子体质谱法。
食品安全国家标准
食品接触材料及制品 锌迁移量的测定
1 范围
本标准规定了食品接触材料及其制品在食品模拟物中浸泡后锌迁移量测定的火焰原子吸收光谱
法、电感耦合等离子体发射光谱法、电感耦合等离子体质谱法和二硫腙比色法。
本标准适用于食品接触材料及其制品中锌迁移量的测定。
第一法 火焰原子吸收光谱法
2 原理
采用食品模拟物浸泡食品接触材料及制品中预期与食品接触的部分,浸泡液用火焰原子吸收光谱
仪进行测定,以213.9nm处吸收强度与其质量浓度的定量关系,测定样品中锌的含量。
3 试剂和材料
除非另有说明,本方法所用试剂均为优级纯,水为GB/T 6682规定的二级水。
3.1 试剂
3.1.1 硝酸(HNO3)。
3.1.2 配制食品模拟物所需试剂:依据GB 31604.1的规定。
3.2 试剂配制
3.2.1 食品模拟物:按照GB 5009.156的规定配制。
3.2.2 硝酸溶液(1+1):量取500mL硝酸,加至500mL水,混匀。
3.2.3 硝酸溶液(5+95):吸取5mL硝酸,用水稀释至100mL。
3.3 标准品
氧化锌(ZnO,CAS号:1314-13-2):纯度>99.99%,或经国家认证并授予标准物质证书的一定浓度
的锌标准溶液。
3.4 标准溶液配制
3.4.1 锌标准储备液(1000mg/L):准确称取1.2447g(精确至0.0001g)氧化锌,加少量硝酸溶液(1
+1),加热溶解,移入1000mL容量瓶,加水至刻度。混匀。
3.4.2 锌标准中间液(10.0mg/L):吸取锌标准储备液1.00mL于100mL容量瓶中,加硝酸溶液(5+
95)至刻度,混匀。
GB 31604.42-2016
GB
NATIONAL STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
National standard for food safety -
Determination of zinc migration quantity in
food contact materials and products
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the
People’s Republic of China
3. No action is required - Full-copy of this standard will be automatically &
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope ... 4
Method I Flame atomic absorption spectrometry ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 5
5 Analytical procedures ... 6
6 Expression of analysis results ... 6
7 Precision... 7
8 Others ... 7
Method II Inductively coupled plasma atomic emission spectrometry ... 7
Method III Inductively coupled plasma mass spectrometry ... 7
Method IV Dithizone colorimetry ... 7
9 Principle... 7
10 Reagents and materials... 7
11 Instruments and equipment ... 10
12 Analytical procedures ... 10
13 Expression of analysis results ... 11
14 Precision ... 12
15 Others ... 12
Annex A Reference conditions for flame atomic absorption spectrometry ... 13
Foreword
The determination of zinc migration quantity in GB/T 5009.72-2003 Method for
analysis of hygienic standard of aluminum-wares for food use, GB/T 5009.64-
2003 Method for analysis of hygienic standard of rubber sheet (ring) for food
use, GB/T 5009.65-2003 Method for analysis of hygienic standard of rubber
sealing ring for pressure cooker for food use, GB/T 5009.66-2003 Method for
analysis of hygienic standard of nipple of a feeding bottle, GB/T 5009.79-2003
Hygienic analytical method of rubber hose for food use and SN/T 2829-2011
Food contact materials for export - Metal materials - Determination of migrant
heavy metals in food simulant - Inductively coupled plasma atomic emission
spectrometric method is substituted by this Standard.
Compared with GB/T 5009.72-2003, the major changes in this Standard are as
follows.
— MODIFY the standard name as “National standard for food safety -
Determination of zinc migration quantity in food contact materials and
products”;
— ADD the flame atomic absorption spectrometry;
— ADD the inductively coupled plasma atomic emission spectrometry; and
— ADD the inductively coupled plasma mass spectrometry.
National standard for food safety -
Determination of zinc migration quantity in food
contact materials and products
1 Scope
This Standard specifies the flame atomic absorption spectrometry, inductively
coupled plasma atomic emission spectrometry, inductively coupled plasma
mass spectrometry, and dithizone colorimetry for the determination of zinc
migration quantity in food contact materials and their products after immersed
in food simulant.
This Standard is applicable to the determination of zinc migration quantity in
food contact materials and their products.
Method I Flame atomic absorption spectrometry
2 Principle
USE food simulant to immerse the sections expected to be in contact with the
food in the food contact materials and products. USE a flame atomic absorption
spectrometer to determine the soaking solution. DETERMINE the content of
intensity and its mass concentration at 213.9nm.
3 Reagents and materials
Unless otherwise indicated, the reagents and water used in this method are
guaranteed reagents and Type II reagent grade water specified in GB/T 6682,
respectively.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Reagents needed for the preparation of food simulant. in accordance
with the provisions of GB 31604.1.
The absolute difference between two independent determination results under
repetitive conditions shall not exceed 10% of the arithmetic mean.
8 Others
The method detection limit is 0.02mg/L. The limit of quantitation is 0.06mg/L.
Method II Inductively coupled plasma atomic emission
spectrometry
SEE GB 31604.49.
Method III Inductively coupled plasma mass spectrometry
SEE GB 31604.49.
9 Principle
After the sample is soaked, zinc ion and dithizone form a magenta complex at
the pH of 4.0 to 5.5. DISSOLVE in carbon tetrachloride. ADD sodium thiosulfate
to prevent copper, mercury, lead, silver and cadmium ion interference.
COMPARE with the standard series for quantitation.
10 Reagents and materials
Unless otherwise indicated, the reagents and water used in this method are
analytical reagents and Type III reagent grade water specified in GB/T 6682,
respectively.
10.1.1 Glacial acetic acid (CH3COOH). guaranteed reagent.
10.1.2 Nitric acid (HNO3). guaranteed reagent.
10.2.10 Methyl orange indicator (2g/L). WEIGH 0.2g of methyl orange. USE
ethanol to dissolve to the volume of 100mL.
10.2.11 Acetic acid - acetate buffer solution. WEIGH same amount of acetic
acid solution (2mol/L) and sodium acetate solution (2mol/L) for mixture. The pH
of this solution is about 4.7. USE dithizone - carbon tetrachloride solution
(0.1g/L) for several extractions. 10mL each time. REMOVE the zinc until the
green color on the carbon tetrachloride layer remains the same. DISCARD the
dithizone in acetic acid - acetate buffer solution, until carbon tetrachloride
becomes colorless. DISCARD the carbon tetrachloride layer.
10.2.12 Sodium thiosulfate solution (250g/L). WEIGH 25g of sodium
thiosulfate. ADD 60mL of water. USE acetic acid solution (2mol/L) to adjust the
pH to 4.0 to 5.5. ADD water to 100mL. USE dithizone - carbon tetrachloride
solution (0.1g/L) to extract several times. 10mL each time. REMOVE the zinc
until the green color on the carbon tetrachloride layer remains the same.
DISCARD the carbon tetrachloride layer. USE carbon tetrachloride to extract
the excessive dithizone in acetic acid - acetate buffer solution, until carbon
10.2.13 Dithizone - carbon tetrachloride working solution. DRAW 1mL of
dithizone - carbon tetrachloride solution (0.1g/L). ADD carbon tetrachloride to
10mL. MIX evenly. USE a 1cm cuvette. USE carbon tetrachloride to adjust the
zero point. DETERMINE the absorbance (A) at a wavelength of 520nm.
CALCULATE the number of milliliters (V) of dithizone - carbon tetrachloride
solution (0.1g/L) required for the preparation of 100mL of dithizone - carbon
tetrachloride working solution (57% transmittance) according to the Formula (1).
DRAW VmL of dithizone - carbon tetrachloride solution (0.1g/L). USE carbon
tetrachloride to dilute to 100mL.
Zinc oxide (ZnO, CAS number. 1314-13-2). Zinc standard solution with the
purity of greater than 99.99%, or a certain concentration of zinc standard
solution certified by China and granted the Reference Material Certificate.
10.4 Standard solution preparation
10.4.1 Zinc standard stock solution (1 000mg/L). Accurately WEIGH 1.244 7g
of zinc oxide. ADD small amount of nitric acid solution (1 + 1). HEAT for
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