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食品安全国家标准 食品接触材料及制品 异氰酸酯的测定
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GB 31604.45-2016
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标准编号: GB 31604.45-2016 (GB31604.45-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 异氰酸酯的测定
英文名称: Food contact materials for export -- Polymer materials -- Determination of isocyanates by high performance liquid chromatography
行业: 国家标准
中标分类: X09
字数估计: 8,842
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2741-2010; GB/T 23296.22-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.45-2016: 食品安全国家标准 食品接触材料及制品 异氰酸酯的测定
GB 31604.45-2016 英文名称: Food contact materials for export -- Polymer materials -- Determination of isocyanates by high performance liquid chromatography
1 范围
本标准规定了食品接触材料用塑料及其制品中甲苯-2,6-二异氰酸酯、二苯基甲烷-4,4'-二异氰酸
酯、甲苯-2,4-二异氰酸酯、萘-1,5-二异氰酸酯、苯基异氰酸酯、六亚甲基二异氰酸酯、环己基异氰酸酯和以上7种异氰酸酯总量的测定方法。
本标准适用于聚氨酯塑料及其制品中甲苯-2,6-二异氰酸酯、二苯基甲烷-4,4'-二异氰酸酯、甲苯-2,4-二异氰酸酯、萘-1,5-二异氰酸酯、苯基异氰酸酯、六亚甲基二异氰酸酯、环己基异氰酸酯和以上7种异氰酸酯总量的检测。
2 原理
试样中异氰酸酯经二氯甲烷振荡提取后,与9-N-甲氨甲基蒽进行衍生反应,衍生产物采用C18液相色
谱柱分离,荧光检测器测定,外标法定量。
3 试剂和材料
除非另有说明,所有试剂均为分析纯,水为GB/T 6682规定的一级水。
3.1 试剂
3.1.1 二氯甲烷(CH2Cl2):5A分子筛干燥过夜,备用。
3.1.2 乙醚(C2H6O)。
3.1.3 磷酸(HPO3)。
3.1.4 乙腈(C2H3N):色谱纯。
3.1.5 N,N-二甲基甲酰胺(C3H7NO):纯度大于99%。
3.1.6 三乙胺(C6H15N)。
3.1.7 9-N-甲氨甲基蒽(C16H15N):纯度大于99%。
3.2 试剂配制
3.2.1 衍生试剂(260mg/L):称取9-N-甲氨甲基蒽0.013g,用二氯甲烷溶解并转移至50mL容量瓶
中,用二氯甲烷定容,避光保存。现用现配。
3.2.2 衍生物溶剂:量取50mLN,N-二甲基甲酰胺于100mL容量瓶中,加入40mL乙腈,用水定容。
3.2.3 三乙胺溶液(3%,体积分数):在1L容量瓶中,加入30mL三乙胺,用水定容。
3.2.4 缓冲溶液:在1L容量瓶中,加入950mL3%三乙胺溶液(3%,体积分数),用磷酸调节pH至3,
用水定容。
3.3 标准品
3.3.1 甲苯-2,6-二异氰酸酯(C9H6N2O2,CAS号:91-08-7):纯度大于98%。
3.3.2 二苯基甲烷-4,4'-二异氰酸酯(C15H10N2O2,CAS号:101-68-8):纯度大于98%。
3.3.3 甲苯-2,4-二异氰酸酯(C9H6N2O2,CAS号:584-84-9):纯度大于98%。
3.3.4 萘-1,5-二异氰酸酯(C12H6N2O2,CAS号:3173-72-6):纯度大于98%。
3.3.5 苯基异氰酸酯(C7H5ON,CAS号:103-71-9):纯度大于98%。
3.3.6 环己基异氰酸酯(C7H11ON,CAS号:3173-53-3):纯度大于98%。
3.3.7 六亚甲基二异氰酸酯(C8H12O2N2,CAS号:822-06-0):纯度大于98%。
3.4 标准溶液配制
3.4.1 异氰酸酯储备液(1000mg/L):称取各种异氰酸酯标准物质0.01g(精确到0.1mg),二氯甲烷
溶解后转移至10mL容量瓶中,二氯甲烷定容。储备液-20℃避光干燥保存,有效期为1个月。
3.4.2 异氰酸酯标准中间液(100mg/L):分别量取5mL二氯甲烷于6个10mL容量瓶中,分别移入
1.0mL各种异氰酸酯储备液,二氯甲烷定容。标准中间液-20℃避光干燥保存,有效期为1个月。
3.4.3 异氰酸酯标准工作液(1mg/L):分别量取5mL二氯甲烷于6个10mL容量瓶中,分别移入100μL
各异氰酸酯标准中间液,二氯甲烷定容,混匀。标准工作液-20℃避光干燥保存,有效期为2周。
3.4.4 混合异氰酸酯标准工作液:分别量取5mL二氯甲烷于6个10mL容量瓶中,依次移入0.00mL、
0.01mL、0.05mL、0.10mL、0.25mL、0.50mL各异氰酸酯标准中间液,二氯甲烷定容,混匀,得到各异
氰酸酯浓度均分别为0.0mg/L、0.10mg/L、0.50mg/L、1.0mg/L、2.5mg/L、5.0mg/L的混合标准工
作液。该混合标准工作液-20℃避光干燥保存,有效期为2周。
4 仪器和设备
4.1 液相色谱仪:配置荧光检测器。
4.2 玻璃瓶:20mL,配聚四氟乙烯瓶盖;使用前应干燥。
4.3 水相滤膜:0.45μm。
4.4 pH计。
4.5 分析天平:感量0.0001g和0.01g。
5 分析步骤
5.1 试样前处理
称取1g(精确到0.01g)剪碎后的试样(面积不大于1cm×1cm),放入20mL玻璃瓶中,加入10mL
二氯甲烷和1mL衍生试剂,密封,避光,振荡12h,提取液转移至另一20mL玻璃瓶中,密封,-20℃下保
存。剩余样品残渣重复提取衍生12h,合并提取液,氮气浓缩至干,加入10mL衍生物溶剂,超声溶解,
0.45μm滤膜过滤,待上机测定。
5.2 测定
5.2.1 色谱条件
a) 色谱柱:C18柱,柱长150mm,内径4.6mm,粒径5μm或等效柱;
b) 流动相:A为乙腈;B为缓冲溶液,洗脱梯度见表1;
5.2.2 标准曲线的制作
分别量取1mL各浓度混合标准工作液于6个20mL玻璃瓶中,再分别加入10mL二氯甲烷和1mL
衍生试剂,密封,避光反应30min,氮气浓缩至干,再加入10mL衍生物溶剂,超声溶解,0.45μm滤膜
过滤,按5.2.1的色谱条件进行测定,以试样中各种异氰酸酯浓度为横坐标,以各异氰酸酯衍生物色谱
峰峰面积为纵坐标,绘制标准工作曲线,得到线性方程。异氰酸酯标准溶液衍生物色谱图见附录A。
5.2.3 测定
按照5.2.1的色谱条件,对5.1中的待测液进行测定。根据各异氰酸酯衍生物保留时间,确定试样
中异氰酸酯的种类。根据各异氰酸酯衍生物色谱峰峰面积,由标准曲线计算出样液中异氰酸酯单体量。
6 分析结果的表述
6.1 异氰酸酯的计算
结果保留两位有效数字。
6.2 异氰酸酯总量的计算
异氰酸酯总量[以异氰酸根(NCO)计]按式(2)计算:
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
本方法中甲苯-2,6-二异氰酸酯、二苯基甲烷-4,4'-二异氰酸酯、甲苯-2,4-二异氰酸酯、萘-1,5-二异氰酸酯、苯基异氰酸酯、环己基异氰酸酯和六亚甲基二异氰酸酯的检出限为0.03mg/kg,定量限为0.1mg/kg。
GB 31604.45-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact
Materials and Articles - Determination of Isocyanate
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 Instrument and equipment . 6
5 Analysis steps . 7
6 Expression of the analysis results .. 8
7 Precision . 9
8 Others . 9
6 Expression of the analysis results .. 8
7 Precision . 9
8 Others . 9
Foreword
This Standard replaces GB/T 23296.22-2009 "Food contact materials - Determination
of isocyanates in plastics - High performance liquid chromatography" AND SN/T 2741-
2010 "Food contact materials for export - Polymer materials - Determination of
isocyanates by high performance liquid chromatography".
Compared with GB/T 23296.22-2009 AND SN/T 2741-2010, main changes of this
Standard are as follows.
- Modify the Standard name to "National food safety standard - Food contact
materials and articles - Determination of isocyanate";
- Increase the number of analyte to 7;
- Cancel the preparation of blank samples;
- Modify the matrix standard curve to the standard-solution’s standard curve;
- Modify the expression of the analysis results.
National Food Safety Standard - Food Contact
Materials and Articles - Determination of Isocyanate
1 Scope
This Standard specifies the determination methods for toluene-2,6-diisocyanate,
diphenylmethane-4,4'-diisocyanate, toluene-2,4-diisocyanate, naphthalene-1,5-
diisocyanate, phenyl isocyanate, hexamethylene diisocyanate and cyclohexyl
isocyanate in plastics for food contact material and their products; this Standard
specifies the determination method for the total amount of the above 7 isocyanates.
This Standard applies to the detection of toluene-2,6-diisocyanate, diphenylmethane-
4,4'-diisocyanate, toluene-2,4-diisocyanate, naphthalene-1,5-diisocyanate, phenyl
isocyanate, hexamethylene diisocyanate and cyclohexyl isocyanate in polyurethane
plastics and their products; this Standard applies to the detection of the total amount
of the above 7 isocyanates.
2 Principle
In the sample, after isocyanate is vibrated-extracted by dichloromethane, isocyanate
starts derivative reaction with 9-N-methylaminomethyl hydrazine. The derivatized
products are separated by C18 liquid chromatography column, determined by
fluorescence detector AND quantified by external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents shall be the analytically pure. The water shall
be the Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Dichloromethane (CH2Cl2). it shall be dried by 5A molecular sieves, stay for
overnight for standby application.
3.1.2 Ethyl ether (C2H6O).
3.1.3 Phosphoric acid (HPO3).
3.1.4 Acetonitrile (C2H3N). chromatographic purity.
3.4 Preparation of the standard solution
3.4.1 Isocyanate stock solution (1000 mg/L). weigh and take 0.01 g (accurate to 0.1
mg) of various isocyanate standard materials; dissolve the dichloromethane; then
transfer it to a volumetric flask of 10 mL; dilute the dichloromethane to the constant
volume. Stock solution shall be stored at -20 °C under dry preservation; it shall be kept
from the light. The term of validity is 1 month.
3.4.2 Standard intermediate-solution of isocyanate (100 mg/L). respectively weigh and
into various 1.0 mL of isocyanate stock solution; dilute them to the constant volume
with dichloromethane. The standard intermediate-solution shall be stored at -20 °C
under dry preservation; it shall be kept from the light. The term of validity is 1 month.
3.4.3 Standard working solution of Isocyanate (1 mg/L). respectively weigh and take
5mL of dichloromethane into six 10mL volumetric flasks; respectively add 100 μL of
various standard intermediate-solutions of isocyanate; dilute them to the constant
volume with dichloromethane; mix them evenly. Standard working solution shall be
stored at -20 °C under dry preservation; it shall be kept from the light. The term of
validity is 2 weeks.
mL of dichloromethane into six 10 mL volumetric flasks; successively add 0.00 mL,
0.01 mL, 0.05 mL, 0.10 mL, 0.25 mL and 0.50 mL of various standard intermediate-
solutions of isocyanate; dilute them to the constant volume with dichloromethane; mix
them evenly; the mixed standard working solutions whose isocyanate’s concentration
are respectively 0 mg/L, 0.10 mg/L, 0.50 mg/L, 1.0 mg/L, 2.5 mg/L and 5.0 mg/L can
be acquired. These mixed standard working solutions shall be stored at -20 °C under
dry preservation; they shall be kept from the light. The term of validity is 2 weeks.
4 Instrument and equipment
4.1 Liquid chromatograph. configure the fluorescence detector.
4.3 Aqueous filter membrane. 0.45 μm.
4.4 pH meter.
4.5 Analytical balance. the sensitivity shall be 0.0001 g and 0.01 g.
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