摘要
采用红外光谱、液相色谱-质谱联用技术和高分辨率质谱对间苯三酚法制备TATB的胺化废水中的副产物1-氨基-3,5-二乙氧基-2,4,6-三硝基苯(AETB)进行了定性鉴定。利用高效液相色谱建立了AETB的含量分析方法,确定了最佳实验条件,并采用外标法对此方法进行了检验。结果表明,色谱条件为:C18柱(250mm×4.6mm,5μm),流动相为乙腈-水(体积比85∶15),检测波长为224nm,进样量为10μL。外标法中所得峰面积与AETB的质量浓度呈线性关系,线性相关系数为0.999 8。该方法操作简单,无需对样品进行前处理,实验所得结果准确合理,可作为制备TATB产生的胺化废水中1-氨基-3,5-二乙氧基-2,4,6-三硝基苯残留量测定的方法。
The by-product 1-amino-3,5-diethoxy-2,4,6-trinitrobenzene（AETB）in the amination wastewater of TATB prepared with m-trihydroxybenzene method was qualitatively identified by IR spectroscopy,liquid chromatography-mass spectrometry and high resolution mass spectroscopy.A HPLC method was established for the quantitative determination of AETB.The optimum experimental conditions were determined and the external standard method was used to test the method.The results show that chromatographic conditions are determined as： C18 column （250mm × 4.6mm,5μm）,mobile phase of acetonitrile/ water with volume ratio of 85：15,detection wavelength 224nm and injection quantity 10μL.A linear relationship was presented between the peak area and the content of AETB by external standard method,and the linear correlation coefficient is 0.9998.This method has the advantages of simple operation and without pretreatment of the samples,and experimental result is accurate and reasonable,which can be used to detect residue quantity of AETB in the wastewater of TATB.
作者
于宪峰
周群
王伯周
YU Xian-feng ZHOU Qun WANG Bo-zhou(Unit 63961 of PLA,Beijing 100012 ,China Xi＇an Modern Chemistry Research Institute, Xi＇an 710065, China)
出处
《火炸药学报》
EI
CAS
CSCD
北大核心
2017年第2期37-40,46,共5页
Chinese Journal of Explosives & Propellants
基金
国家自然科学基金(No.21373157)
关键词
TATB
AETB
高效液相色谱
外标法
耐热炸药
TATB
1-amino-3,5-ethoxy-2,4,6- trinitrobenzene （AETB）
high performance liquid chromatography（HPLC）
external standard method
heat-resistant explosive
