Qualitative and quantitative investigation of organophosphates in an electrochemically and thermally treated lithium hexafluorophosphate-based lithium ion battery electrolyte by a developed liquid chromatography-tandem quadrupole mass spectrometry method

Author(s): Vadim Kraft ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Waldemar Weber ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Benjamin Streipert ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Ralf Wagner ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Carola Schultz ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Martin Winter ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵ , Sascha Nowak ¹ ^, ² ^, ³ ^, ⁴ ^, ⁵

Publication date (Electronic): 2016

Journal: RSC Advances

Publisher: Royal Society of Chemistry (RSC)

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Abstract

The work focused on the development of a new liquid chromatography-tandem quadrupole mass spectrometry method for the identification and quantification of organophosphates in lithium hexafluorophosphate-based lithium ion battery electrolytes.

Abstract

The presented work was focused on the development of a new liquid chromatography-tandem quadrupole mass spectrometry method (LC-MS/MS) for the identification and quantification of organophosphates in lithium hexafluorophosphate (LiPF ₆)-based lithium ion battery electrolytes. The investigated electrolyte consists of 1 M LiPF ₆ dissolved in ethylene carbonate/ethyl methyl carbonate (50/50, wt%) and was treated electrochemically and thermally. For the electrochemical experiments, the cut-off potential in the half cells was held at 5.5 V for 72 h. The thermal degradation experiments were performed in aluminum vials at 95 °C for a period of 13 days. In the first part of this work, an already established gas chromatography-mass spectrometry (GC-MS) method for identification of dimethyl fluorophosphates (DMFP) and diethyl fluorophosphate (DEFP) was applied. In the second part, the LC-MS/MS method including determination of characteristic transitions in a product ion scan was developed. The developed method was applied for the identification of various analytes in the decomposed electrolytes. In addition, a possible formation of ionic and non-ionic OPs based on findings of this work and our previous reports is presented. In the third and final part, a quantification study of DMFP and DEFP was performed with a newly developed LC-MS/MS method and compared with results obtained by GC-MS. In addition, trimethyl phosphate (TMP) and triethyl phosphate (TEP) were quantified. These studies included the investigation of the suppression effects caused by the sample matrix during the application of the LC-MS/MS method.