Determination of sulfur and selenium in environmental samples by ICP-OES and ICP-MS

Jiří Čmelík



Abstract


Inductively coupled plasma optical emission spectrometry is method which enables to determine total
content of various elements in the periodic table. My work is aim for coupling of ICP-OES, as
element specific detector, with vapour generation system. This coupling enables separation of
analyte from matrix and determination of form of element which can be transforming to gaseous
phase. This is demonstrated on examples of determination of sulfane in water samples, determination
of free and total sulfur dioxide in wine and determination of Se^IV in algae Chlorella. Hydrogen
sulfide and acid volatile sulfides in water were transformed, by acidification to gaseous phase and
subsequently detected by ICP-OES. The proposed method provides results comparable to iodometric
titration in the tested concentration range 0,06-22,0 mg/l. Limit of detection for the
determination  of hydrogen sulfide by this method is 0,03 mg/l. Determination of free and total
sulfur dioxide is based on releasing of gaseous sulfur dioxide by addition of acid, sulfur from
SO[2] is measured by ICP-OES. Free SO[2] is released from sample by acidification, total SO[2] can
be determined after hydrolysis of bond forms by sodium hydroxide.

 Second part is aim for fractionation of selenium in algae Chlorella. For this purposes simple
fractionation scheme were arrange. This scheme is consist of extraction steps, which enclosed
extraction by water, extraction by SDS, extraction by isopropanol/chloroform mixture. In extracts
was selenium determined by ICP-MS method. Further speciation analyses of selenium in algea
chlorella were performed by LC-ICP-MS method.