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Optimization of internal standard selection for precise trace impurity quantification in Li2S via ICP-OES.

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Title: Optimization of internal standard selection for precise trace impurity quantification in Li2S via ICP-OES.
Authors: Lee, Woomi1 (AUTHOR), Ryu, Kwang-Sun1 (AUTHOR) ryuks@ulsan.ac.kr
Source: JAAS (Journal of Analytical Atomic Spectrometry). Jul2026, Vol. 41 Issue 7, p2352-2359. 8p.
Subjects: Matrix effect, Trace element analysis, Solid state batteries, Lithium compounds, Inductively coupled plasma atomic emission spectrometry, Analytical chemistry
Abstract: Lithium sulfide (Li2S) is a critical precursor for sulfide-based solid electrolytes in next-generation all-solid-state batteries; accordingly, rigorous control and accurate quantification of trace-level impurities are essential. Accurate determination by inductively coupled plasma optical emission spectrometry (ICP-OES) is, however, severely complicated by matrix-induced signal suppression and enhancement in high-concentration Li2S solutions. This study systematically evaluated the selection of internal standards (IS) to compensate for matrix effects and improve analytical precision in a 1% (w/v) Li2S matrix. Five IS candidates, namely Sc, Y, Ru, Bi, and In, were screened on the basis of total excitation energy levels and assessed for matrix-correction efficiency across 16 target analytes. Method performance was validated through recovery, method detection limits (MDLs), and limits of quantification (LOQs). Without IS correction, matrix-induced signal depression reduced analyte recoveries to as low as 38.7%; implementation of an optimized IS scheme restored quantitative accuracy and markedly narrowed inter-replicate variability. Sc (361.383 nm) and Y (324.225 nm) demonstrated the broadest corrective efficacy, whereas Ru (240.272 nm) caused systematic overcorrection, up to 164% recovery for low-excitation-energy elements, due to its high total excitation energy (12.52 eV). IS-corrected MDLs were substantially lower than those obtained by EC. These findings establish total excitation energy matching as the governing criterion for IS selection in complex lithium-based matrices. [ABSTRACT FROM AUTHOR]
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Database: Engineering Source
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Abstract:Lithium sulfide (Li2S) is a critical precursor for sulfide-based solid electrolytes in next-generation all-solid-state batteries; accordingly, rigorous control and accurate quantification of trace-level impurities are essential. Accurate determination by inductively coupled plasma optical emission spectrometry (ICP-OES) is, however, severely complicated by matrix-induced signal suppression and enhancement in high-concentration Li2S solutions. This study systematically evaluated the selection of internal standards (IS) to compensate for matrix effects and improve analytical precision in a 1% (w/v) Li2S matrix. Five IS candidates, namely Sc, Y, Ru, Bi, and In, were screened on the basis of total excitation energy levels and assessed for matrix-correction efficiency across 16 target analytes. Method performance was validated through recovery, method detection limits (MDLs), and limits of quantification (LOQs). Without IS correction, matrix-induced signal depression reduced analyte recoveries to as low as 38.7%; implementation of an optimized IS scheme restored quantitative accuracy and markedly narrowed inter-replicate variability. Sc (361.383 nm) and Y (324.225 nm) demonstrated the broadest corrective efficacy, whereas Ru (240.272 nm) caused systematic overcorrection, up to 164% recovery for low-excitation-energy elements, due to its high total excitation energy (12.52 eV). IS-corrected MDLs were substantially lower than those obtained by EC. These findings establish total excitation energy matching as the governing criterion for IS selection in complex lithium-based matrices. [ABSTRACT FROM AUTHOR]
ISSN:02679477
DOI:10.1039/d6ja00119j