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Characterisation of the phosgene response of a membrane inlet ~(63)Ni ion mobility spectrometer

机译:膜入口〜(63)Ni离子迁移谱仪的光气响应特性

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摘要

A membrane inlet ~(63)Ni ion mobility spectrometer interfaced to a quadrupole mass spectrometer with permeation, exponential dilution approaches and syringe-based systems were used to characterise the ion mobility spectrometry (IMS) response to phosgene in dry air (water concentration less than 16.5 mg m~(-3)). Phosgene produced a principle product ion in the negative mode with a reduced mobility of 2.16 cm~2 V~(-1) s~(-1), with an unresolved artefact at higher concentrations having a reduced mobility of 2.32 cm~2 V~(-1) s~(-1). The limit of detection of the system with a membrane inlet fitted was estimated to be less than 1 mg m~(-3), with an upper limit to the dynamic range of 32 mg m~(-3). Mass spectrometric data indicated the existence of [(H_2O)_nCl]~-, [(H_2O)_nCl_2]~-, [(H_2O)_nCl]~-, [(H_2O)nCl]~-,and [(H_2O)_n(CO_2)Cl]~-. The existence of two possible mechanisms for product ion formation is proposed: dissociative electron capture, as well as hydrolysis followed by electron capture. The effect on water contamination of the drying media within the ion mobility spectrometer was also investigated, and the effects were similar to those observed previously with studies on chlorine. Reduced mobility of the product ions was observed to decrease with increasing water contamination of the drying media used within the instrument, while limits of detection increased slightly to less than 2.4 mg m~(-3), with no significant effect on dynamic ranges of response or resolution. Preliminary results also indicated a positive mode response for phosgene, albeit at significantly higher concentrations to those observed in the negative mode.
机译:膜入口〜(63)Ni离子迁移谱仪与具有渗透,指数稀释方法和基于注射器的系统的四极质谱仪相连接,用于表征离子迁移谱(IMS)对干燥空气中光气的响应(水浓度小于16.5 mg m〜(-3))。光气在负模态下产生主要产物离子,其迁移率降低了2.16 cm〜2 V〜(-1)s〜(-1),在较高浓度时存在未分解的伪影,迁移率降低了2.32 cm〜2 V〜(-1) (-1)秒〜(-1)。装有膜入口的系统的检测极限估计小于1 mg m〜(-3),动态范围的上限为32 mg m〜(-3)。质谱数据表明存在[(H_2O)_nCl]〜-,[(H_2O)_nCl_2]〜-,[(H_2O)_nCl]〜-,[(H_2O)nCl]〜-和[(H_2O)_n( CO_2)Cl]〜-。提出了两种可能的产物离子形成机理:解离电子俘获,以及水解然后电子俘获。还研究了离子迁移谱仪中干燥介质对水污染的影响,其影响与先前对氯的研究相似。观察到产物离子迁移率的降低随仪器中使用的干燥介质的水污染的增加而降低,而检出限则略微提高到小于2.4 mg m〜(-3),对动态响应范围没有显着影响或分辨率。初步结果也表明光气具有正模式响应,尽管其浓度明显高于在负模式下观察到的浓度。

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