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Coupling of microwave induced plasma optical emission spectrometry with HPLC separation for speciation analysis of Cr(III)/Cr(VI)

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Abstract

Feasibility and limitations of direct coupling of high performance liquid chromatographic (HPLC) separation to microwave induced plasma (MIP)-optical emission spectrometry (OES) for elementspecific detection was tested and compared to inductively coupled plasma (ICP)-optical emission spectrometric detection on the basis of the Cr(III)/Cr(VI) speciation analysis of water samples. Coupling was performed by a hydraulic high pressure nebulizer (HHPN) radiative-heating/watercooling interface which provides about 20 % and 80 % aerosol yield in the case of helium and argon carrier gases, respectively. Desolvation efficiency of aqueous solutions was approximately 80 %. Applying the ion-pair HPLC separation, the organic eluents and reagents in the MIP cause a 50–75 % signal suppression for Cr(VI) and 25–50 % for Cr(III). In a pure aqueous solution the MIP Cr(VI) signal was by 20 % lower than that of Cr(III). These effects were lower using the ICP source, but they cannot be neglected. Easily ionizable matrix elements (Na, Ca) can cause 70 % signal suppression in the MIP, and 20 % in the ICP. Therefore, species dependent calibration is required in both cases. In the case of HPLC detection by MIP-OES, the detection limit was 13 ng for Cr(III), and 18 ng for Cr(VI). Using the ICP-OES detection, the detection limit was 0.2 ng for Cr (III) and 0.4 ng for Cr (VI). The linear dynamic ranges in both cases were two orders of magnitude.

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Correspondence to G. Heltai.

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Presented at the XVIIIth Slovak Spectroscopic Conference, Spišská Nová Ves, 15–18 October 2006.

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Heltai, G., Fehér, B. & Horváth, M. Coupling of microwave induced plasma optical emission spectrometry with HPLC separation for speciation analysis of Cr(III)/Cr(VI). Chem. Pap. 61, 438–445 (2007). https://doi.org/10.2478/s11696-007-0059-7

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  • DOI: https://doi.org/10.2478/s11696-007-0059-7

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