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食品安全国家标准 食品接触材料及制品 镍迁移量的测定
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GB 31604.33-2016
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标准编号: GB 31604.33-2016 (GB31604.33-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 镍迁移量的测定
英文名称: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of Migration of Nickel
行业: 国家标准
中标分类: X09
字数估计: 8,839
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 5009.81-2003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 31604.33-2016: 食品安全国家标准 食品接触材料及制品 镍迁移量的测定
GB 31604.33-2016 英文名称: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of Migration of Nickel
1 范围
本标准规定了食品接触材料及制品在食品模拟物中浸泡后镍迁移量测定的石墨炉原子吸收光谱
法、电感耦合等离子体质谱法、电感耦合等离子体发射光谱法和丁二酮肟比色法。
本标准适用于食品接触材料及制品中镍迁移量的测定。
第一法 石墨炉原子吸收光谱法
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,浸泡液经石墨炉原子化,在
232.0nm处测定的吸收值在一定浓度范围内与镍含量成正比,与标准系列比较定量。
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 磷酸二氢铵(NH4H2PO4)。
3.1.3 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 硝酸溶液(1+1):量取250mL硝酸,加入250mL水中,混匀。
3.2.2 硝酸溶液(5+95):量取50mL硝酸,加入950mL水中,混匀。
3.2.3 食品模拟物:按照GB 5009.156的规定配制。
3.2.4 磷酸二氢铵溶液(20g/L):称取2.0g磷酸二氢铵,用水溶解,定容至100mL。
3.3 标准品
金属镍(Ni,CAS号:7440-02-0):纯度≥99.99%,或经国家认证并授予标准物质证书的标准溶液。
3.4 标准溶液配制
3.4.1 镍标准储备液(1000mg/L):准确称取1g金属镍(精确至0.001g),加少量硝酸溶液(1+1),加
热直至镍完全溶解,然后转入1000mL容量瓶,加水至刻度,混匀。或采用经国家认证并授予标准物质
证书的标准溶液稀释。
3.4.2 镍标准中间液(10.0mg/L):吸取镍标准储备液1.00mL于100mL容量瓶中,加硝酸溶液(5+
95)稀释至刻度,混匀。
3.4.3 镍标准使用液(1.00mg/L):吸取镍标准储备液10.0mL于100mL容量瓶中,加硝酸溶液(5+
95)稀释至刻度,混匀。
3.4.4 镍标准系列溶液:准确吸取镍标准使用液(1.00mg/L)0mL、0.500mL、1.00mL、2.00mL、
3.00mL、4.00mL分别置于50mL容量瓶中,用相应食品模拟物稀释至刻度,混匀,浓度为0μg/L、
10.0μg/L、20.0μg/L、40.0μg/L、60.0μg/L、80.0μg/L。
注:可根据仪器的灵敏度、线性范围以及样液中镍实际含量确定标准系列溶液中镍的浓度和范围。若所选食品模拟物为中性或碱性,则需添加适量硝酸使该溶液中硝酸浓度约为5%(体积分数)。
4 仪器和设备
注:所有玻璃器皿均需用硝酸溶液(1+5)浸泡过夜,用水冲洗干净备用。
4.1 原子吸收光谱仪:配石墨炉原子化器,镍空心阴极灯。
4.2 分析天平:感量0.1mg。
5 分析步骤
5.1 试样的预处理
根据待测样品的预期用途和使用条件,按照GB 5009.156和GB 31604.1规定的迁移试验方法及试
验条件进行迁移试验。浸泡液经充分混匀后,取部分浸泡试液用于分析。若浸泡试液为中性或碱性,则
添加适量硝酸使试液中硝酸浓度约为5%(体积分数)。同时做试样空白试验。
5.2 测定
5.2.1 仪器测试条件
仪器参考条件见表A.1。
5.2.2 标准曲线的制作
按浓度由低到高的顺序分别吸取10μL镍标准系列溶液和5μL磷酸二氢铵溶液(20g/L)(可根据
所使用的仪器确定最佳进样量)同时注入石墨炉中,经原子化后测定其吸光值,以标准系列浓度为横坐
标,对应的吸光值为纵坐标绘制标准曲线。
5.2.3 试样测定
在与测定标准溶液相同的试验条件下,吸取10μL样品溶液和5μL磷酸二氢铵溶液(20g/L)(可
根据所使用的仪器确定最佳进样量)同时注入石墨炉中,经原子化后测定其吸光度值,与标准系列比较
定量。同时测试试样空白溶液。
6 分析结果的表述
由标准曲线得到试样溶液中镍的浓度,扣除空白值后按GB 5009.156进行迁移量计算,得到食品接
触材料及制品中镍的迁移量。计算结果保留三位有效数字。
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20%。
8 其他
本方法检出限为1μg/L,定量限为3μg/L。
第二法 电感耦合等离子体质谱法
见GB 31604.49。
第三法 电感耦合等离子体发射光谱法
见GB 31604.49。
第四法 丁二酮肟比色法
9 原理
食品模拟物试液中的镍在弱碱性条件下,与丁二酮肟反应生成红色络合物,用三氯甲烷萃取。向三
氯甲烷萃取液中加入稀盐酸反萃取,向稀盐酸萃取液中加入溴水,再加氨水脱色,然后与碱性丁二酮肟
反应生成红色络合物,与标准系列比较定量。
10 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规定的三级水。
10.1 试剂
10.1.1 枸橼酸氢二铵[(NH4)2HC6H5O7]。
10.1.2 丁二酮肟[(CH3)2C2(NOH)2]。
10.1.3 乙醇(C2H5OH)。
10.1.4 三氯甲烷(CHCl3)。
10.1.5 溴水(Br2)。
10.1.6 氢氧化钠(NaOH)。
10.1.8 氨水(NH3·H2O)。
10.1.9 硝酸(HNO3):优级纯。
10.1.10 配制食品模拟物所需试剂:依据GB 31604.1的规定。
10.2 试剂配制
10.2.1 枸橼酸氢二铵溶液(100g/L):称取10g枸橼酸氢二铵溶于水至100mL。
10.2.2 乙醇溶液(95+5):向95mL乙醇中加入5mL水,混匀。
10.2.3 丁二酮肟乙醇溶液(10g/L):称取1g丁二酮肟溶于100mL乙醇溶液(95+5)中,混匀。如有
不溶解物,过滤,滤液备用。
10.2.4 氢氧化钠溶液(0.2mol/L):称取1.0g氢氧化钠溶于125mL水中。
混匀。
10.2.6 氢氧化钠溶液(20%):称取20g氢氧化钠用水定容至100mL。
10.2.7 盐酸溶液(0.5mol/L):量取20.9mL盐酸,用水稀释至500mL,混匀。
10.2.8 氨水溶液(5mol/L):量取33.8mL氨水,用水稀释至100mL,混匀。
10.2.9 氨水溶液(2mol/L):量取13.5mL氨水,用水稀释至100mL,混匀。
10.2.10 氨水溶液(0.3mol/L):量取20.3mL氨水,用水稀释至1000mL,混匀。
10.2.11 硝酸溶液(1+1):量取100mL硝酸,缓慢加入100mL水中,混匀。
10.2.12 硝酸溶液(5+95):量取10mL硝酸,缓慢加入190mL水中,混匀。
10.2.13 食品模拟物:按照GB 5009.156的规定配制。
金属镍(Ni,CAS号:7440-02-0):纯度≥99.99%,或经国家认证并授予标准物质证书的标准溶液。
10.4 标准溶液配制
10.4.1 镍标准储备液(1000mg/L):准确称取1g金属镍(精确至0.001g),加少量硝酸溶液(1+1),
加热直至镍完全溶解,然后转入1000mL容量瓶,加水至刻度,混匀。或采用经国家认证并授予标准物
质证书的标准溶液稀释。
10.4.2 镍标准使用液(10.0mg/L):吸取镍标准储备液(1000mg/L)1.00mL于100mL容量瓶中,加
硝酸溶液(5+95)稀释至刻度,混匀。
11 仪器和设备
注:所有玻璃器皿均需用硝酸溶液(1+5)浸泡过夜,用水冲洗干净备用。
11.2 分析天平:感量0.1mg。
12 分析步骤
12.1 试样的预处理
同5.1。
12.2 测定
12.2.1 标准曲线的制作
分别吸取镍标准使用液(10.0mg/L)0mL、0.250mL、0.500mL、1.00mL、2.00mL、3.00mL、
4.00mL、5.00mL至100mL容量瓶中,加食品模拟物定容至刻度,对应的浓度系列为0μg/L、
25.0μg/L、50.0μg/L、100μg/L、200μg/L、300μg/L、400μg/L、500μg/L。加氢氧化钠溶液(20%)调
数滴氨水溶液(2mol/L)调溶液pH为8~9。加2mL丁二酮肟乙醇溶液(10g/L),加10mL三氯甲
烷,剧烈振摇1min,静置,将三氯甲烷分离至60mL分液漏斗中。向水层加三氯甲烷5mL按上述操
作反复进行两次,合并三氯甲烷液,弃去水层。用10mL氨水溶液(0.3mol/L)洗涤三氯甲烷层,剧烈
振摇30s,静置,分离三氯甲烷层于另一60mL分液漏斗中,向该漏斗中加10mL盐酸溶液(0.5mol/L),剧
烈振摇1min,静置,分离三氯甲烷层于另一分液漏斗中;加5mL盐酸溶液(0.5mol/L)同上操作,合并
盐酸液,移入25mL具塞比色管中,加2mL溴水,振摇。静置1min,加氨水溶液(5mol/L)至无色,再
多加2mL氨水溶液(5mol/L),在流水中冷至室温;加2mL碱性丁二酮肟溶液(10g/L),加水至
25mL充分混合,放置20min,于540nm处测定吸光度。以吸光度为纵坐标,标准浓度为横坐标,绘制
标准曲线。
GB 31604.33-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products
Determination of nickel migration
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
Table of Contents
Foreword . 3
1 Scope .. 4
2 Principle . 4
3 Reagents and materials . 4
4 Instruments and equipment .. 6
5 Analysis procedure .. 6
6 Expression of analysis results .. 7
7 Precision . 7
8 Others . 7
9 Principle . 7
10 Reagents and materials . 8
11 Instruments and equipment .. 10
12 Analysis procedure . 10
13 Expression of analysis results . 11
14 Precision . 11
15 Others . 11
Annex A Reference temperature rise program of graphite furnace atomic
absorption spectrometer . 12
Foreword
This Standard replaces the determination method for nickel migration in GB/T
5009.81-2003 “Method for analysis of hygienic standard of stainless steel food
containers and table wares” 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”.
Compared with the determination method for nickel in GB/T 5009.81-2003, the
main changes are as follows.
- MODIFY the standard name TO “National food safety standard - Food
contact materials and products - Determination of nickel migration”;
- ADD Inductively coupled plasma mass spectrometry and inductively
coupled plasma atomic emission spectrometry.
National food safety standard -
Food contact materials and products
Determination of nickel migration
1 Scope
This Standard specifies the graphite furnace atomic absorption spectrometry,
inductively coupled plasma mass spectrometry, inductively coupled plasma
atomic emission spectrometry and spectrophotometric method using
dimethylglyoxime for the determination of nickel migration in food contact
materials and products after being soaked in food simulants.
This Standard applies to the determination of nickel migration in food contact
materials and products.
Method I -- Graphite furnace atomic absorption spectrometry
2 Principle
Use food simulants to soak parts of food contact materials and products that
are expected to come in contact with foods. The soaking solution is atomized
in a graphite furnace. The absorbance measured at 232.0 nm is proportional to
the nickel content within a certain concentration range, which is compared with
the standard series to quantify.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all guarantee
reagents, and the water is grade-2 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Nitric acid (HNO3).
3.1.2 Ammonium dihydrogen phosphate (NH4H2PO4).
3.1.3 Reagents for preparing food simulants. According to specifications of GB
31604.1.
4 Instruments and equipment
NOTE. All glassware must be soaked in nitric acid solution (1 + 5) overnight and rinsed
4.1 Atomic absorption spectrometer. equipped with graphite furnace atomizer,
nickel hollow cathode lamp.
4.2 Analytical balance. with a division of 0.1 mg.
5 Analysis procedure
5.1 Pretreatment of samples
According to the expected use and the use conditions of the sample to be tested,
carry out the migration test in accordance with the migration test methods and
test conditions specified in GB 5009.156 and GB 31604.1. After the soaking
solution is thoroughly mixed, take part of the soaking solution for analysis. If the
so that the concentration of nitric acid in the test solution is about 5 % (volume
fraction). At the same time carry out the sample blank test.
5.2 Determination
5.2.1 Instrument test conditions
Instrument reference conditions are shown in Table A.1.
5.2.2 Plotting of standard curves
PIPETTE 10 μL of nickel standard solution and 5 μL of ammonium dihydrogen
phosphate solution (20 g/L) (the optimal injection volume may be determined
in accordance with the instrument used) in the order of concentration from low
atomization, MEASURE the absorbance value. Take the concentrations of the
standard series as the abscissa and take the corresponding absorbance values
as the ordinate to plot the standard curve.
5.2.3 Determination of samples
Under the same test conditions as those for the determination of standard
solution, PIPETTE 10 μL of sample solution and 5 μL of ammonium dihydrogen
phosphate solution (20 g/L) (the optimal injection volume may be determined
in accordance with the instrument used), INJECT them into the graphite furnace
at the same time. After atomization, MEASURE the absorbance value.
complexes, which are compared with the standard series to quantify.
10 Reagents and materials
Unless otherwise stated, the reagents used in this method are all analytical
reagents, the water is the grade-3 water specified in GB/T 6682.
10.1 Reagents
10.1.1 Diammonium hydrogen nitrite [(NH4)2HC6H5O7].
10.1.2 Dimethylglyoxime [(CH3)2C2(NOH)2].
10.1.3 Ethanol (C2H5OH).
10.1.4 Chloroform (CHCl3).
10.1.6 Sodium hydroxide (NaOH).
10.1.7 Hydrochloric acid (HCl).
10.1.8 Ammonia (NH3 · H2O).
10.1.9 Nitric acid (HNO3). excellent regent.
10.1.10 Reagents for preparing food simulants. according to the specifications
of GB 31604.1.
10.2 Preparation of reagents
10.2.1 Diammonium hydrogen nitrite solution (100 g/L). WEIGH 10 g of
diammonium hydrogen nitrite and DISSOLVE in water to 100 mL.
well.
10.2.3 Dimethylglyoxime ethanol solution (10 g/L). DISSOLVE 1 g of
dimethylglyoxime and DISSOLVE in 100 mL of ethanol solution (95 + 5), MIX
well. If there is any insoluble material, filter and the filtrate is for later use.
10.2.4 Sodium hydroxide solution (0.2 mol/L). DISSOLVE 1.0 g of sodium
hydroxide in 125 mL of water.
10.2.5 Basic dimethylglyoxime solution (10 g/L). WEIGH 1 g of
11 Instruments and equipment
NOTE. All glassware must be soaked in nitric acid solution (1 + 5) overnight and rinsed
11.1 Spectrophotometer. with 1 cm cuvette.
11.2 Analytical balance. with a division of 0.1 mg.
12 Analysis procedure
12.1 Pretreatment of samples
The same as subclause 5.1.
12.2 Determination
12.2.1 Plotting of standard curves
Respectively PIPETTE 0 mL, 0.250 mL, 0.500 mL, 1.00 mL, 2.00 mL, 3.00 mL,
4.00 mL, 5.00 mL of nickel standard use solution (10.0 mg/L) to 100-mL
concentration series are 0 μg/L, 25.0 μg/L, 50.0 μg/L, 100 μg/L, 200 μg/L, 300
μg/L, 400 μg/L and 500 μg/L. ADD sodium hydroxide solution (20 %) to adjust
to neutral or weak alkaline, LET STAND for 2 h, FILTER, TRANSFER the filtrate
into a 250-mL separatory funnel, ADD 2 mL of diammonium hydrogen nitrite
solution (100 g/L), ADD a few drops of ammonia solution (2 mol/L) to adjust the
solution pH to 8 ~ 9. ADD 2 mL of dimethylglyoxime ethanol solution (10 g/L),
ADD 10 mL of chloroform, vigorously SHAKE for 1 min, LET STAND,
SEPARATE chloroform into a 60-mL separatory funnel. ADD 5 mL of chloroform
to the aqueous layer and REPEAT the above operations twice, COMBINE
solution (0.3 mol/L) to wash the chloroform layer, vigorously SHAKE for 30 s,
LET STAND, SEPARATE the chloroform layer into another 60-mL separatory
funnel; ADD 10 mL of hydrochloric acid solution (0.5 mol/L) to the funnel,
vigorously SHAKE for 1 min, LET STAND, SEPARATE the chloroform layer into
another separatory funnel. ADD 5 mL of hydrochloric acid solution (0.5 mol/L)
and operate as above, COMBINE the hydrochloric acid solution, TRANSFER
to a 25-mL colorimetric tube with stopper, ADD 2 mL of bromine water, SHAKE.
LET STAND for 1 min, ADD ammonia solution (5 mol/L) until colorless, ADD 2
mL of ammonia solution (5 mol/L), COOL to room temperature in running water.
MIX thoroughly, LET STAND for 20 min. DETERMINE the absorbance at 540
nm. TAKE the absorbance as the ordinate and the standard concentration as
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