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Evaluation of different plasma conditions and resolutions for understanding elemental organophosphorus analysis via GC-ICP-SF-MS
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2018-05-11 00:00:00 , DOI: 10.1039/c8ja00092a
Yannick Philipp Stenzel 1, 2, 3, 4 , Martin Winter 1, 2, 3, 4, 5 , Sascha Nowak 1, 2, 3, 4
Affiliation  

The state-of-the-art electrolyte in lithium ion battery application is composed of a solvent mixture of organic carbonates and lithium hexafluorophosphate (LiPF6) as the conducting salt. Decomposition reactions of the hexafluorophosphate anion with the organic carbonates and trace amounts of water in the system result in a large variety of organofluorophosphates. The toxicity of organofluorophosphates has been known for some time and is now drawing interest in the battery research context. Molecular standards are not available as these compounds are supposedly highly toxic, generally unknown or just recently described. Therefore, in this study, the organophosphates formed were investigated with gas chromatography-inductively coupled plasma-sector field-mass spectrometry (GC-ICP-SF-MS). With this setup, it was possible to overcome the need for molecular standards and to perform quantification after separation of species using only one external standard. Comprehensive data of the phosphorus signals were evaluated in different resolution modes (R > 300 and R > 4000) and under different plasma conditions (wet and dry). Thereby, possible interferences originating from aerosol entry, GC solvents, sample matrix or decomposition products could be detected and evaluated. The developed phosphorus speciation procedures and tuning techniques were interrelated. Detection and quantification limits were determined for all setups and additionally, preliminary qualitative and quantitative investigations of different commercially available electrolytes after thermal treatment are presented.

中文翻译:

评估不同的血浆条件和分辨率,以通过GC-ICP-SF-MS 了解元素有机磷的分析

锂离子电池应用中的最新电解质由有机碳酸盐和六氟磷酸锂(LiPF 6)作为导电盐。六氟磷酸根阴离子与有机碳酸酯的分解反应和系统中的痕量水会导致产生各种各样的有机氟磷酸根。有机氟磷酸盐的毒性已经知道了一段时间,现在引起了电池研究的兴趣。分子标准尚不可用,因为这些化合物被认为具有剧毒,通常未知或刚刚被描述。因此,在本研究中,通过气相色谱-电感耦合等离子体扇区场质谱(GC-ICP-SF-MS)对形成的有机磷酸盐进行了研究。通过这种设置,可以克服对分子标准品的需求,并且仅使用一种外标就可以在分离物种后进行定量。R > 300和R > 4000),并且在不同的等离子体条件下(干湿)。因此,可以检测和评估源自气溶胶进入,GC溶剂,样品基质或分解产物的可能干扰。发达的磷形态形成程序和调谐技术是相互联系的。确定了所有设置的检测和定量极限,此外,还介绍了热处理后对不同市售电解质的初步定性和定量研究。
更新日期:2018-05-11
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