| 气相色谱法测定橡胶中的苯胺类物质含量 |
| Determination of Aniline Content in Rubber by Gas Chromatography |
| 投稿时间：2021-03-22 修订日期：2021-03-22 |
| DOI：10.12136/j.issn.1000-890X.2022.08.0629 |
| 中文关键词: 气相色谱 橡胶 苯胺类物质 含量 测定 |
| 英文关键词: gas chromatography rubber anilines content determination |
| 基金项目:国家质量监督检验检疫总局科研项目（2016IK038）；福州海关科研项目（FK2020-27）；福建出入境检验检疫局科技项目（FK2013-42） |
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| 中文摘要: |
| 研究气相色谱法测定橡胶中的苯胺、邻苯二胺、N-乙基苯胺和N，N-二乙基对苯二胺的含量。优化测定步骤如下：准确称取2.0 g试样，加入10 mL乙醇，在25～30 ℃下涡旋振荡10 min，再超声提取20 min，过滤，重复提取1次，合并滤液，用固相萃取柱净化滤液，净化液旋转蒸发至约0.5 mL，用正己烷定容至2 mL，用孔径0.45 μm有机相滤膜过滤；采用HP-5色谱柱，在初始温度50 ℃保持2 min后，以4 ℃·min-1速率升温至170 ℃并保持5 min，再以40 ℃·min-1速率升温至280 ℃并保持2 min的升温程序下进行滤液的气相色谱测试。该方法苯胺、N-乙基苯胺、邻苯二胺和N，N-二乙基对苯二胺的检出限分别为0.005，0.260，0.005和0.005 mg·kg-1，加标回收率为89.00%～110.51%，相对标准偏差为1.61%～9.94%。 |
| 英文摘要: |
| The contents of aniline，N-ethylaniline，o-phenylenediamine and N，N-diethyl-pphenylenediamine
in rubber was determined by gas chromatography. The optimized determination steps were
as follows：accurately weighed 2.0 g of the sample was firstly mixed with 10 mL of ethanol；the mixture
was vortex oscillated for 10 min at 25～30 °C，the obtained solution was ultrasonic extracted for 20 min and
filtered，and the extraction procedure was repeated one more time；the filtrates were then combined，
purified with the solid-phase extraction column；the purified solution was condensed to about 0.5 mL by
rotary evaporation，diluted to 2 mL with n-hexane，and filtered with the organic phase filter film having
an average pore diameter of 0.45 μm；the filtered solution was tested by gas chromatography using a HP-5
chromatographic column，the initial temperature was kept at 50 °C for 2 min，and then the temperature
was raised to 170 °C at a rate of 4 °C·min-1 and held for 5 min，and then heated to 280 °C at a rate of 40
°C·min-1 and maintained for 2 min. The detection limits of aniline，N-ethylaniline，o-phenylenediamine and
N，N-diethyl-p-phenylenediamine in this method were 0.005，0.260，0.005 and 0.005 mg·kg-1 respectively，
the spiked recovery rate was 89.00%～110.51%，and the relative standard deviation was 1.61%～9.94%. |
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