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Application of direct analysis in real time to study chemical vapor generation mechanisms: reduction of dimethylarsinic(V) acid with aqueous NaBH4 under non-analytical conditions.
Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2020-09-04 , DOI: 10.1007/s00216-020-02896-y
Enea Pagliano 1 , Massimo Onor 2 , Zoltan Mester 1 , Alessandro D'Ulivo 2
Affiliation  

The aqueous-phase reaction of dimethylarsinc acid (DMAs(V)) with NaBH4 (THB) was studied under non-analytical conditions (1000 μg/mL As, 0.1 M HCl, 1% NaBH4) with the aim of identifying intermediates and reaction products. The use of direct analysis in real time (DART) with high-resolution mass spectrometry (HRMS), in combination with two different chemical vapor generation systems, allowed the identification of some species not detected by GC-MS such as Me2As–AsMe–AsMe2 and the arsonium species [Me3As–AsMe2]+ and [Me2As–AsMe2–AsMe2]+. Many other methylated species of arsenic containing up to four arsenic atoms have been observed. Unfortunately, the oxidation mechanism that took place in the DART source interfered with the identification of some of those species formed in solution following THB reduction. The species identified by DART-HRMS, together with those previously identified by GC-MS (Me2AsH, Me2AsOH, Me3As, Me3AsO, Me2AsAsMeH, Me2AsAsMe2, and Me2As–O–AsMe2)‚ enabled the formulation of hypotheses on the possible reaction pathways and revealed an aqueous-phase reactivity of DMAs(V) which could not be explained on the basis of current knowledge.



中文翻译:

实时直接分析在研究化学蒸汽产生机理中的应用:在非分析条件下,用NaBH4水溶液还原二甲基ar(V)酸。

在非分析条件(1000μg/ mL As,0.1 M HCl,1%NaBH 4)的非分析条件下研究了二甲基砷酸(DMAs(V))与NaBH 4(THB)的水相反应,目的是鉴定中间体和反应产物。结合两种不同的化学气相生成系统,结合使用高分辨率实时质谱(HRMS)和实时实时直接分析(DART),可以鉴定GC-MS未检测到的某些物种,例如Me 2 As–AsMe –AsMe 2和砷物种[Me 3 As–AsMe 2 ] +和[Me 2 As–AsMe 2 –AsMe 2 ] +。已经观察到许多其他甲基化的砷,最多包含四个砷原子。不幸的是,在DART源中发生的氧化机理干扰了THB还原后溶液中形成的某些物种的鉴定。通过DART-HRMS识别的物种,以及之前通过GC-MS识别的物种(Me 2 AsH,Me 2 AsOH,Me 3 As,Me 3 AsO,Me 2 AsAsMeH,Me 2 AsAsMe 2和Me 2 As–O– AsMe 2)使得能够在可能的反应路径上提出假设,并揭示了DMAs(V)的水相反应性,而这在目前的知识基础上是无法解释的。

更新日期:2020-09-05
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