Rapid and selective determination of free chlorine in aqueous solution using electrophilic addition to styrene by gas chromatography/mass spectrometry

We developed a rapid and selective method for determination of free chlorine in aqueous solution by gas chromatography/mass spectrometry for the first time. Free chlorine was converted to styrene chlorohydrin using electrophilic addition to styrene in sodium acetate buffer solution (pH 5). The chlor...

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Bibliographic Details
Published in:Talanta (Oxford) 2013-01, Vol.103, p.81-85
Main Authors: Wakigawa, Kengo, Gohda, Akinaga, Fukushima, Sunao, Mori, Takeshi, Niidome, Takuro, Katayama, Yoshiki
Format: Article
Language:English
Subjects:
Aqueous solutions
Bleaching Agents - analysis
Buffer solutions
Calibration
Chlorine
Chlorine - analysis
Chlorohydrin
Chlorohydrins - chemistry
Derivatives
Disinfectants - analysis
Electrophilic addition
Forensic science
Free chlorine
Gas chromatography
Gas Chromatography-Mass Spectrometry
GC/MS
Humans
Japan
Limit of Detection
Mass spectrometry
Styrene - chemistry
Styrenes
Water - analysis
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Summary:We developed a rapid and selective method for determination of free chlorine in aqueous solution by gas chromatography/mass spectrometry for the first time. Free chlorine was converted to styrene chlorohydrin using electrophilic addition to styrene in sodium acetate buffer solution (pH 5). The chlorine derivative obtained was extracted with chloroform, and then analyzed by GC/MS. The calibration curve showed good linearity from 0.2–100μg/mL (as available chlorine). The detection limit was 0.1μg/mL, and the intra- and interday accuracy were measured at concentrations of 10, 50, and 75μg/mL to be −1.3 to 6.9% (intraday) and 3.8–8.0% (interday) as % Bias. The precision was between 1.4 and 4.5% as % RSD. These results indicate that this method is a superior technique for the identification of free chlorine. This method was successfully applied to quantification in commercial samples and in samples of a criminal case. ► A rapid and selective method for free chlorine by GC/MS was established for the first time. ► Free chlorine was converted into styrene chlorohydrin. ► This method was successfully applied to commercial samples and samples obtained in an actual criminal case.
ISSN:0039-9140
1873-3573
DOI:10.1016/j.talanta.2012.10.011