文章摘要
Determination of Aniline Content in Rubber by Gas Chromatography
Received:March 22, 2021  Revised:March 22, 2021
DOI：10.12136/j.issn.1000-890X.2022.08.0629
Key Words: gas chromatography；rubber；anilines；content；determination
Author NameAffiliationE-mail
YIN Honglei 1.Rongcheng customs comprehensive technical service center
2.Fuzhou Customs Technology Center 		21558049@qq.com 
DAI Jinlan* Fuzhou Customs Technology Center 21558049@qq.com 
CHENG Lijun Fuzhou Customs Technology Center  
TU Mandi Fuzhou Customs Technology Center  
ZHOU Lei Tianjin Customs  
YＵ Lingyun Chengdu Customs Technology Center  
CHEN Xuecan Rongcheng customs comprehensive technical service center  
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Abstract:
      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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