Abstract

The analysis method based on high performance liquid chromatography (HPLC) is an important tool for the quality control of energetic materials. 1,1'-Diamino-4,4',5,5'-tetranitro-2,2'-biimidazole (DATNBI) as a new low-sensitivity and high-energy explosive, has many potential applications in both civil and military areas. However, the method based on HPLC is not known for the analysis of DATNBI. In this study, a HPLC method has been developed and validated for DATNBI. After the optimization of chromatographic conditions, a reversed-phase HPLC method has been established by using phenyl-hexyl column (4.6 × 150 mm, 3.5 µm) with the detection wavelength of 230 nm. The retention time of DATNBI is 10.37 min with the resolution of all peaks over 2.10. Meanwhile, the method has been also validated and displayed good accuracy, precision, stability and robustness for the analysis of DATNBI. The linear range of DATNBI analysis is 1.0–200 µg·mL⁻¹ with the detection limit of 0.05 µg·mL⁻¹. Further, this method had been applied to the analysis of real DATNBI. The purity of DATNBI was increased from 90.06 to 98.85% after the recrystallization for two times. This study indicates that the HPLC method is fast, efficient, sensitive and accurate for the analysis of DATNBI, and thus it can be used for the quality control of DATNBI.

摘要

基于高效液相色谱（HPLC）的分析方法是高能材料质量控制的重要工具。1,1'-二氨基-4,4'，5,5'-四硝基-2,2'-联咪唑（DATNBI）作为一种新型的低敏高能炸药，在民用和军事领域均具有许多潜在应用。然而，基于HPLC的方法对于DATNBI的分析是未知的。在这项研究中，已经开发出一种HPLC方法，并已针对DATNBI进行了验证。优化色谱条件后，通过使用检测波长为230 nm的苯基己基色谱柱（4.6×150 mm，3.5 µm）建立了反相HPLC方法。DATNBI的保留时间为10.37分钟，所有峰的分离度均超过2.10。同时，该方法也得到了验证，并显示出良好的准确性，精密度，DATNBI分析的稳定性和鲁棒性。DATNBI分析的线性范围是1.0–200 µg·mL^-1的检出限为0.05 µg·mL ^-1。此外，该方法已应用于实际DATNBI的分析。重结晶两次后，DATNBI的纯度从90.06增加到98.85％。这项研究表明，HPLC方法对DATNBI的分析是快速，高效，灵敏和准确的，因此可用于DATNBI的质量控制。