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Phase pure triacetone triperoxide: The influence of ionic strength, oxidant source, and acid catalyst

机译:相纯三丙酮三过氧化物:离子强度,氧化剂来源和酸催化剂的影响

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摘要

The explosive triacetone triperoxide (TATP) is produced by the acid-catalyzed reaction of hydrogen peroxide and acetone, and methods for its identification are important in forensic and military scenarios. Previous work has documented concomitant crystalline polymorphism of the crude reaction product. Here, we have investigated the crystalline phases resulting from TATP syntheses from aqueous hydrogen peroxide as well as from sodium percarbonate and urea peroxide as oxidant sources, under different concentrations and types of acid. Powder X-ray diffraction (PXRD) patterns of the as-prepared powders indicate that, in contrast to previously published conditions, rapid precipitations afford a pure crystalline phase of TATP. High concentrations of Br?nsted acid lead to the selective formation of a single kinetic crystalline phase, while a Lewis acid (SnCl_4) gives rise to a pure specimen of the thermodynamic phase. Additionally, this study highlights the utility of PXRD as a rapid and high-confidence identification tool for TATP which has only now become feasible due to the fairly recent disclosure of crystal structures of the various TATP crystalline polymorphs.
机译:爆炸性三丙酮三氧化二氧(TATP)是由酸催化的过氧化氢和丙酮反应生成的,其鉴别方法在法医和军事场合中很重要。先前的工作已记录了粗反应产物的伴随结晶多态性。在这里,我们研究了在不同浓度和类型的酸下,由过氧化氢水溶液以及过碳酸钠和过氧化脲作为氧化剂来源的TATP合成所产生的结晶相。所制备粉末的粉末X射线衍射(PXRD)图谱表明,与先前公开的条件相比,快速沉淀提供了TATP的纯结晶相。高浓度的布朗斯台德酸导致选择性形成单个动力学结晶相,而路易斯酸(SnCl_4)产生纯的热力学相样品。此外,这项研究强调了PXRD作为TATP的快速和高可信度识别工具的实用性,由于各种TATP晶体多晶型物的晶体结构的最新披露,这种方法直到现在才变得可行。

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