Detailed impurity profiling of graphene oxide fractions by robust inductively coupled plasma optical emission spectrometry monitoring

Poimenova, I.A.; Zhukova, E.Y.; Ovseenko, S.T.; Saratovsky, N.S.; Kiryukhin, I.K.; Ratova, D.V.; Filatov, D.M.; Alekseeva, A.M.; Smirnova, S.V.; Proskurnin, M.A.; Mikheev, I.V.

Авторы: Poimenova Iuliia A., Zhukova Elizaveta Yu, Ovseenko Svetlana T., Saratovsky Nikita S., Kiryukhin Ivan K., Ratova Daria-Mariia V., Filatov Dmitrii M., Alekseeva Anastasia M., Smirnova Svetlana V., Proskurnin Mikhail A., Mikheev Ivan V.
Журнал: Analytica Chimica Acta
Год издания: 2026
Издательство: Elsevier BV
Местоположение издательства: Netherlands
Первая страница: 345140
DOI: 10.1016/j.aca.2026.345140
Аннотация: Background Graphene oxide (GO) is widely used in biomedicine and biotechnology due to its aqueous dispersibility and potential nanozyme activity. However, it remains analytically challenging because of structural heterogeneity and metallic inclusions, which affect its functional performance. GO therefore requires precise trace metal analysis, as even minor compositional variations can be critical. Modern multi-element analysis demands results that are both reliable and accurate, yet sound laboratory practice is not always followed. Although ICP-OES offers high sensitivity and precision, metrological rigor is often lacking. This work addresses the need for validated and robust elemental analysis of GO bulk material and particle-size fractions. Results ICP-OES was employed to quantify metals in bulk GO and to characterize Mn and Ti distribution in GO fractions. A fast algorithm was developed to identify robust plasma conditions by mapping the Mermet coefficient (Mg II/Mg I intensity ratio) across a range of flow rates and RF power levels. Concentrations for selected elements in the bulk material ranged from 10–1 to 103 mg kg–1; in aqueous dispersions, values reached up to 103 mg L–1. Validation parameters for Mn, Ti, and Fe included recoveries of 85–115%, detection limits of 0.1–0.3 ng kg–1 (for used weight ca. 50 mg), and intra-/inter-day RSDs not exceeding 7%. The Mermet coefficient exhibited an RSD of ∼0.6%, indicating minimal matrix interference. Fraction analysis revealed a monotonic decrease in Mn toward fractions with smaller lateral-size cut-offs. ATR-FTIR spectra were obtained for stirred, purified, and ultrasound-treated GO fractions to assess whether purification altered the surface functional groups. Significance This study provides a validated approach for trace metal analysis in GO, combining sensitivity, robustness, and reproducibility across both bulk solid and aqueous dispersion forms. By experimentally examining the influence of plasma conditions on analytical performance, it offers the first systematic assessment of GO-specific ICP-OES parameter optimization. The results support more reliable characterization of GO materials and enable improved quality control in applications where elemental composition critically affects functionality.
Добавил в систему: Михеев Иван Владимирович

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