University of Oulu

Suvela, R., Genevrais, S., Niemelä, M. et al. The effect of experimental conditions on the formation of dixanthogen by triiodide oxidation in the determination of ethyl xanthate by HPLC–ICP-MS/MS. ANAL. SCI. 38, 1221–1231 (2022).

The effect of experimental conditions on the formation of dixanthogen by triiodide oxidation in the determination of ethyl xanthate by HPLC–ICP-MS/MS

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Author: Suvela, Ronja1; Genevrais, Simon2; Niemelä, Matti1;
Organizations: 1Research Unit of Sustainable Chemistry, University of Oulu, P.O Box 3000, 90014, Oulu, Finland
2University of Poitiers, Poitiers, France
Format: article
Version: published version
Access: open
Online Access: PDF Full Text (PDF, 1.9 MB)
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Language: English
Published: Springer Nature, 2022
Publish Date: 2022-08-31


The rising concern over the environmental impact of xanthates, especially in the arctic region, has increased the need to study these traditional flotation reagents in greater detail. The environmental concern relates mostly to the formation of carbon disulfide (CS₂) and the heavy metal complexes of xanthates. Due to the unstable nature and multiple reaction mechanisms of xanthates, their reliable determination at low concentration levels is difficult. In this study, a xanthate pretreatment method was optimized and applied for the determination of ethyl xanthate (EX⁻) by high performance liquid chromatography–inductively coupled plasma tandem mass spectrometry (HPLC–ICP-MS/MS). Ethyl xanthate was oxidized to diethyl dixanthogen ((EX)₂) by triiodide (I₃⁻) in aqueous solution and the formed (EX)₂ was extracted into n-hexane. Important experimental parameters, including pH, I₃⁻ amount, and oxidation time, were optimized and the detection limit of 0.29 mg L⁻¹ for potassium ethyl xanthate was obtained. During the optimization experiments, it was found that the oxidation reaction resulted in multiple products, decreasing the efficiency of (EX)₂ formation and, therefore, the sensitivity of the method. The proposed method was applied to wastewater samples with recoveries of 105–106%. This study provides a selective method for the determination of ethyl xanthate and introduces novel information on the parameters affecting the oxidation of xanthates.

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Series: Analytical sciences
ISSN: 0910-6340
ISSN-E: 1348-2246
ISSN-L: 0910-6340
Volume: 38
Issue: 9
Pages: 1221 - 1231
DOI: 10.1007/s44211-022-00155-x
Type of Publication: A1 Journal article – refereed
Field of Science: 116 Chemical sciences
Funding: R. Suvela is grateful for the funding provided by the Technology and Natural Sciences Doctoral Programme of the University of Oulu, Oulu, Finland. Open Access funding provided by University of Oulu including Oulu University Hospital.
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