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使用气相色谱 - 质谱联用技术鉴别霍奇登派罗代克斯(®)和三七(®)。

Discriminating Hodgdon Pyrodex(®) and Triple Seven(®) using gas chromatography-mass spectrometry.

作者信息

Routon Benjamin J, Kocher Brandon B, Goodpaster John V

机构信息

Department of Chemistry and Chemical Biology, Forensic and Investigative Sciences Program, Indiana University Purdue University Indianapolis, Indianapolis, IN 46202-3724, USA.

出版信息

J Forensic Sci. 2011 Jan;56(1):194-9. doi: 10.1111/j.1556-4029.2010.01534.x. Epub 2010 Aug 23.

DOI:10.1111/j.1556-4029.2010.01534.x
PMID:20735702
Abstract

Pyrodex(®) and Triple Seven(®) are black powder substitutes that often find use as fillers in improvised explosive devices, such as pipe bombs. These propellants have essentially the same overall appearance and oxidizers, but different fuels. For example, Pyrodex(®) contains sulfur, sodium benzoate, and dicyandiamide (DCDA), whereas Triple Seven(®) lacks sulfur but also contains 3-nitrobenzoic acid. In this method, intact particles and postblast solid residues were reacted with bis(trimethylsilyl)trifluoroacetamide + 1% trimethylchlorosilane in acetonitrile for 30 min at 60°C. The resultant trimethylsilyl derivatives of the organic fuels were then analyzed by gas chromatography-mass spectrometry. Each derivative was clearly resolved from other components, and high-quality mass spectra were obtained. In addition, characteristic fragments resulting from loss of a methyl radical from the molecular ion (m/z 163 for sulfur, m/z 171 for DCDA, m/z 179 for benzoic acid, and m/z 224 for nitrobenzoic acid) were able to be monitored.

摘要

派罗代克斯(Pyrodex®)和三七(Triple Seven®)是黑色火药替代品,常用于简易爆炸装置(如管状炸弹)的填充物。这些推进剂的整体外观和氧化剂基本相同,但燃料不同。例如,派罗代克斯(Pyrodex®)含有硫、苯甲酸钠和双氰胺(DCDA),而三七(Triple Seven®)不含硫,但含有3-硝基苯甲酸。在该方法中,完整颗粒和爆炸后固体残留物与双(三甲基硅基)三氟乙酰胺 + 1% 三甲基氯硅烷在乙腈中于60°C反应30分钟。然后通过气相色谱 - 质谱法分析所得有机燃料的三甲基硅基衍生物。每种衍生物都能与其他成分清晰分离,并获得了高质量的质谱图。此外,能够监测到分子离子失去一个甲基自由基产生的特征碎片(硫的m/z为163,DCDA的m/z为171,苯甲酸的m/z为179,硝基苯甲酸的m/z为224)。

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