Krauss Shannon T, Forbes Thomas P, Jobes Dillon
National Institute of Standards and Technology, Gaithersburg, MD, USA.
Department of Physics and Engineering Physics, Tulane University, New Orleans, LA, USA.
Electrophoresis. 2021 Feb;42(3):279-288. doi: 10.1002/elps.202000279. Epub 2020 Dec 6.
Advancement in rapid targeted chemical analysis of homemade and improvised explosive devices is critical for the identification of explosives-based hazards and threats. Gradient elution moving boundary electrophoresis (GEMBE), a robust electrokinetic separation technique, was employed for the separation and detection of common inorganic oxidizers from frequently encountered fuel-oxidizer mixtures. The GEMBE system incorporated sample and run buffer reservoirs, a short capillary (5 cm), an applied electric field, and a pressure-driven counterflow. GEMBE provided a separation format that allowed for continuous injection of sample, selectivity of analytes, and no sample cleanup or filtration prior to analysis. Nitrate, chlorate, and perchlorate oxidizers were successfully detected from low explosive propellants (e.g., black powders and black powder substitutes), pyrotechnics (e.g., flash powder), and tertiary explosive mixtures (e.g., ammonium nitrate- and potassium chlorate-based fuel-oxidizer mixtures). Separation of these mixtures exhibited detection without interference from a plethora of additional organic and inorganic fuels, enabled single particle analysis, and demonstrated semiquantitative capabilities. The bulk counterflow successfully excluded difficult components from fouling the capillary, yielding estimated limits of detection down to approximately 10 μmol/L. Finally, nitrate was separated and detected from postblast debris collected and directly analyzed from two nitrate-based charges.
快速靶向化学分析自制和简易爆炸装置对于识别基于爆炸物的危险和威胁至关重要。梯度洗脱移动边界电泳(GEMBE)是一种强大的电动分离技术,用于从常见的燃料-氧化剂混合物中分离和检测常见的无机氧化剂。GEMBE系统包括样品和运行缓冲液储液器、短毛细管(5厘米)、施加的电场和压力驱动的逆流。GEMBE提供了一种分离形式,允许连续进样、分析物的选择性,并且在分析前无需样品净化或过滤。从低爆速推进剂(如黑火药和黑火药替代品)、烟火剂(如闪光粉)和第三类爆炸混合物(如硝酸铵和氯酸钾基燃料-氧化剂混合物)中成功检测到了硝酸盐、氯酸盐和高氯酸盐氧化剂。这些混合物的分离显示出检测不受大量其他有机和无机燃料的干扰,能够进行单颗粒分析,并具有半定量能力。大量逆流成功地排除了难溶性成分对毛细管的污染,检测限估计低至约10μmol/L。最后,从两枚基于硝酸盐的炸药收集的爆炸后碎片中分离并检测到了硝酸盐,并进行了直接分析。