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食品安全国家标准 食品接触材料及制品 三乙胺和三正丁胺的测定
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GB 31604.37-2016
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标准编号: GB 31604.37-2016 (GB31604.37-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 三乙胺和三正丁胺的测定
英文名称: Food contact materials for export -- Polymers -- Determination of triethylamine and tributylamine in polycarbonate resin and its products -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 6,641
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2890-2011
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.37-2016: 食品安全国家标准 食品接触材料及制品 三乙胺和三正丁胺的测定
GB 31604.37-2016 英文名称: Food contact materials for export -- Polymers -- Determination of triethylamine and tributylamine in polycarbonate resin and its products -- Gas chromatography
1 范围
本标准规定了食品接触材料及制品中三乙胺和三正丁胺含量的气相色谱测定方法。
本标准适用于聚碳酸酯食品接触材料及制品中三乙胺和三正丁胺含量的测定。
2 原理
样品经二氯甲烷溶解后,加入丙酮使聚合物树脂沉淀,溶液中的三乙胺和三正丁胺经浓缩定容后采
用气相色谱法测定,外标法定量。
3 试剂和材料
除非另有说明,本方法所用试剂均为分析纯。试验中应避免使用塑料材质的容器及转移器具。
3.1 试剂
3.1.1 二氯甲烷(CH2Cl2)。
3.1.2 丙酮(C3H6O)。
3.2 标准品
3.2.1 三乙胺(C6H15N,CAS号:121-44-8):纯度≥99%,或经国家认证并授予标准物质证书的标准
物质。
3.2.2 三正丁胺(C12H27N,CAS号:102-82-9):纯度≥99%,或经国家认证并授予标准物质证书的标准
物质。
3.3 标准溶液配制
3.3.1 标准储备液
在50mL烧杯中准确称取10mg三乙胺和10mg三正丁胺(精确至0.1mg),加入约30mL二氯
甲烷,溶解后定量转移至100mL容量瓶内,用二氯甲烷定容并摇匀,得到标准储备液。标准储备液应
于4℃下密封避光保存,有效期为1个月。
3.3.2 标准工作溶液
移取标准储备液4.00mL,用二氯甲烷稀释至100mL,定容并摇匀。再将稀释后的溶液分别移取
1.00mL、2.00mL、3.00mL、4.00mL、5.00mL于5个不同的20mL容量瓶中,用二氯甲烷定容并摇
匀,得到浓度分别为0.2mg/L、0.4mg/L、0.6mg/L、0.8mg/L、1.0mg/L的标准工作溶液。标准工作
溶液应于临用前配制。
4 仪器和设备
4.1 气相色谱仪:配氮磷检测器。
4.2 分析天平或电子天平:感量0.1mg。
4.3 离心机:3000r/min。
4.4 旋转蒸发仪。
4.5 具塞刻度离心管:2mL或5mL。
4.6 针头式有机相过滤器:0.22μm。
5 分析步骤
5.1 试样制备
先将试样用切割工具将其破碎成粒径小于5mm×5mm后再称量。切割样品时,不可使其发热
变软。
5.2 试样溶液制备
称取1g试样(精确至0.001g)置于200mL锥形瓶中,加入20mL二氯甲烷。待样品完全溶解后,
边摇动锥形瓶边用分液漏斗逐滴加入100mL丙酮。滴加完毕后将瓶内溶液摇匀,离心10min,取上层
清液旋转蒸发浓缩至近1mL。将浓缩液完全转移至具塞刻度离心管中,再用二氯甲烷定容至2.0mL,
得到试样溶液,供气相色谱上机测定。
注1:溶液离心可分次进行,需将离心后的上层清液合并。
注2:若试样溶液中有少量浑浊,可用针头式有机相过滤器过滤后再上气相色谱仪测定。
5.3 空白试验
除不加试样外,采用与5.2完全相同的分析步骤、试剂和用量,进行平行操作。
5.4 气相色谱参考条件
5.4.1 色谱柱:ZB-5石英毛细管柱,柱长30m,内径0.32mm,膜厚5μm,或相当者;
5.4.2 柱温:初始温度40℃,保持5min;然后以20℃/min的速率升至250℃,保持5min;
5.4.3 进样口温度:200℃;
5.4.4 检测器温度:250℃;
5.4.5 载气:氮气(纯度≥99.999%),流量1.0mL/min;
5.4.6 检测器氢气流量:3mL/min;
5.4.7 检测器空气流量:60mL/min;
5.4.8 进样量:1μL;
5.4.9 进样方式:不分流进样。
5.5 标准工作曲线的制作
按照5.4所列色谱条件,对标准工作溶液进行检测。以标准工作溶液中三乙胺和三正丁胺的浓度
(mg/L)为横坐标,以对应的色谱峰面积为纵坐标,进行线性回归,绘制标准工作曲线。
5.6 样液测定
按照5.4所列测定条件,对空白溶液和试样溶液依次进样测定,得到空白溶液和试样溶液中三乙胺
和三正丁胺的色谱峰面积。根据标准曲线得到溶液中三乙胺和三正丁胺的浓度。
6 分析结果的表述
样品中三乙胺和三正丁胺含量按式(1)计算:
计算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试结果的绝对差值不得超过算术平均值的10%。
8 其他
三乙胺和三正丁胺的方法检出限均为0.2mg/kg,定量限均为0.4mg/kg。
GB 31604.37-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard –
Food Contact Materials and Articles –
Determination of Triethylamine and Tributylamine
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 . 5
5 Analysis steps . 5
6 Expression of analysis results .. 7
7 Precision. 7
8 Other . 7
Annex A Gas chromatogram of triethylamine and tributylamine . 8
National Food Safety Standard –
Food Contact Materials and Articles –
Determination of Triethylamine and Tributylamine
1 Scope
This Standard specifies the determination method of triethylamine and
tributylamine by gas chromatography in food contact materials and articles.
This Standard is applicable to the determination of triethylamine and
tributylamine in polycarbonate food contact materials and articles.
2 Principle
After the sample is dissolved in dichloromethane, acetone shall be added to
precipitate the polymer resin. Triethylamine and tri-n-butylamine in solution are
concentrated and weighed, then measured by gas chromatography, and
quantified by external standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all analytically
pure. Plastic containers and transfer equipment shall be avoided during the test.
3.1 Reagents
3.1.1 Dichloromethane (CH2Cl2).
3.1.2 Acetone (C3H6O).
3.2 Standard product
3.2.1 Triethylamine (C6H15N, CAS No.. 121-44-8). a standard substance with
a purity of ≥99% or certified by the state and granted with a standard substance
certificate.
3.2.2 Tributylamine (C12H27N, CAS No.. 102-82-9). a standard substance
with a purity of ≥99% or certified by the state and granted with a standard
substance certificate.
conical flask. After the addition, shake the bottle solution. Centrifuge 10 min.
Take the supernatant and evaporate to a concentration of nearly 1 mL.
Completely transfer the concentrate to a plugged centrifuge tube. Dilute with
dichloromethane and set volume to 2.0 mL. Obtain the sample solution for the
gas chromatography determination.
NOTE 1. The solution centrifugation can be performed in several times. The supernatant after
centrifugation must be merged.
NOTE 2. If there is a small amount of turbidity in the sample solution, it can be filtered by a
needle-type organic phase filter and then measured by gas chromatography.
5.3 Blank test
Except that the sample is not added, use the same analysis steps, reagents
and dosage same as in 5.2 for parallel operation.
5.4 Gas chromatography reference conditions
5.4.1 Chromatographic column. ZB-5 quartz capillary column, column
length of 30m, inner diameter of 0.32mm, film thickness of 5μm, or the
equivalent.
5.4.2 Column temperature. initial temperature of 40°C, hold 5min; then
increase at 20°C/min to 250°C for 5min.
5.4.3 Inlet temperature. 200°C.
5.4.4 Detector temperature. 250°C.
5.4.5 Carrier gas. nitrogen (purity ≥99.999%), flow of 1.0 mL/min.
5.4.6 Detector hydrogen flow rate. 3 mL/min.
5.4.8 Injection volume. 1 μL.
5.4.9 Injection method. split-less injection.
5.5 Making of standard working curve
Inspect the standard working solution according to the chromatographic
conditions listed in 5.4. Take the concentration of triethylamine and
tributylamine (mg/L) in the standard working solution as the abscissa, the
corresponding chromatographic peak area as the ordinate, perform the linear
regression to draw the standard working curve.
5.6 Sample solution determination
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