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Trace detection of perchlorate in industrial-grade emulsion explosive with portable surface-enhanced Raman spectroscopy

机译:便携式表面增强拉曼光谱法检测工业级乳化炸药中的高氯酸盐

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Recent analyses by ion-exchange chromatography (IC) showed that, beside nitrate, the majority of the industrial-grade emulsion explosives, extensively used by most separatists in the southern Thailand insurgency, contained small traces of perchlorate anions. In demand for the faster, reliable, and simple detection methods, the portable detection of nitrate and perchlorate became the great interest for the forensic and field-investigators. This work proposed a unique method to detect the trace amount of perchlorate in seven industrial-grade emulsion explosives under the field tests. We utilized the combination of the portable Raman spectroscope, the developed surfaced-enhanced Raman substrates, and the sample preparation procedures. The portable Raman spectroscope with a laser diode of 785. nm for excitation and a thermoelectric-cooled CCD spectrometer for detection was commercially available. The SERS substrates, with uniformly distributed nanostructured silver nanorods, were fabricated by the DC magnetron sputtering system, based on the oblique-angle deposition technique. The sample preparation procedures were proposed based on (1) pentane extraction technique and (2) combustion technique, prior to being dissolved in the purified water. In comparison to the ion chromatography and the conventional Raman measurements, our proposed methods successfully demonstrated the highly sensitive detectability of the minimal trace amount of perchlorate from five of the explosives with minimal operating time. This work was therefore highly practical to the development for the forensic analyses of the post-blast explosive residues under the field-investigations.
机译:离子交换色谱(IC)的最新分析表明,除硝酸盐外,泰国南部叛乱分子大多数分离主义者广泛使用的大多数工业级乳化炸药还含有少量的高氯酸根阴离子。对于更快,可靠和简单的检测方法的需求,便携式硝酸盐和高氯酸盐的检测成为法医和现场调查人员的极大兴趣。这项工作提出了一种独特的方法,可以通过现场测试来检测7种工业级乳化炸药中的痕量高氯酸盐。我们利用了便携式拉曼光谱仪,开发的表面增强拉曼底物和样品制备程序的组合。便携式拉曼光谱仪具有用于激发的785.nm激光二极管和用于检测的热电冷却CCD光谱仪。基于斜角沉积技术,通过直流磁控溅射系统制备了具有均匀分布的纳米银纳米棒的SERS基板。在溶解于纯净水中之前,基于(1)戊烷提取技术和(2)燃烧技术提出了样品制备程序。与离子色谱法和常规拉曼测量相比,我们提出的方法成功地证明了从五种炸药中以最小的操作时间即可检测到痕量高氯酸盐的痕量的高灵敏度。因此,这项工作对于在现场调查下开发爆炸后爆炸物残留的法医分析非常实用。

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