Pacific Northwest National Laboratory , 902 Battelle Boulevard , Richland , Washington 99352 , United States.
Anal Chem. 2018 Jul 3;90(13):8086-8092. doi: 10.1021/acs.analchem.8b01261. Epub 2018 Jun 14.
Using a commercial mass spectrometer interfaced with an atmospheric flow tube (AFT) allowed for the detection of a variety of inorganic compounds used as oxidizers in homemade explosives (HMEs) at picogram levels. The AFT provides reaction times of between 3 and 5 s with flows of 6 L/min, enabling detection levels, after thermal desorption, similar to those previously demonstrated for RDX vapor in the low parts per quadrillion range. The thermal desorption of chlorate and perchlorate salts resulted in the production of the corresponding anions which have higher electron affinities than that of the nitrate reactant ions. A dielectric barrier discharge, used as the ionization source, produced the nitrate reactant ions. In some instances, the molecular salt formed adducts with the nitrate, chlorate, and/or perchlorate anions, giving insight into the original identity of the salt cation. Urea nitrate, guanidine nitrate, and potassium nitrate were also detected as adducts with the nitrate reactant ion. The direct room-temperature vapor detection of urea nitrate and hydrogen peroxide, which have relatively high vapor pressures compared to the other salts in this study, is also demonstrated. Room-temperature vapor detection of chlorate and perchlorate salts is possible by the addition of a dilute acid which converts the salt into a more volatile acidic form. A discussion of the instrumentation, methods used, and the ionization chemistry is provided.
使用商业质谱仪与大气流动管(AFT)接口,可以在皮克级水平检测到用作自制爆炸物(HME)氧化剂的各种无机化合物。AFT 以 6 L/min 的流速提供 3 到 5 秒的反应时间,实现了热解吸后的检测水平,类似于之前在万亿分之几的低水平范围内对 RDX 蒸汽所展示的水平。氯酸根和高氯酸盐盐的热解吸产生了相应的阴离子,其电子亲和力高于硝酸盐反应物离子。作为电离源的介电阻挡放电产生了硝酸盐反应物离子。在某些情况下,分子盐与硝酸盐、氯酸根和/或高氯酸盐阴离子形成加合物,深入了解盐阳离子的原始身份。尿素硝酸盐、胍硝酸盐和硝酸钾也被检测为与硝酸盐反应物离子的加合物。还证明了室温下对具有相对较高蒸气压的硝酸尿素和过氧化氢的直接蒸汽检测。通过添加稀酸将盐转化为更易挥发的酸性形式,可以实现氯酸盐和高氯酸盐盐的室温蒸汽检测。提供了对仪器、使用的方法和电离化学的讨论。