Abstract
A method for conducting fast and efficient gas chromatography based on short multicapillaries in straight alignment combined with atomic emission detection was developed for field analysis. The strategy enables for speciation analysis of organometallic compounds. The analytes are simultaneously ethylated and preconcentrated on a solid phase microextraction (SPME) fiber placed in the headspace over the sample for 25 min. The ethylated species are then completely separated and selectively quantified within 25 s under isothermal conditions. A new miniaturized speciation analyzer has been constructed and evaluated. The system consists of a GC injection port and a lab-made miniaturized GC unit directly coupled with miniaturized plasma excitation source. The emitted light is transferred via optical fiber and registered with a miniaturized charged coupled device (CCD) based spectrometer. Working parameters for multicapillary column gas chromatography with atomic emission detector, including carrier gas flow rate, desorption temperature, and GC column temperature, were optimized to achieve good separation of analytes. Basic investigations of the fundamental properties of 5 cm-long multicapillary column, to evaluate its potential and limitations as a rapid separation unit, are presented. The adaptation of the technique for use with a SPME system and with a multichannel element-selective plasma-emission detector is highlighted.
Highlights
Gas chromatography is a popular and powerful analytical tool, but often suffers from long analysis times
Multicapillary gas chromatography microwave induced plasma optical emission spectrometry (MCGC-MIP-OES) combined with derivatization to alkyl compounds has been widely employed for speciation analysis of harmful organometallic pollutants
A method based on solid phase microextraction (SPME) in combination with multicapillary gas chromatography column (MCGC) separation and MIP-OES detection was developed and applied for ultra-trace mercury and tin speciation analysis in water samples
Summary
Gas chromatography is a popular and powerful analytical tool, but often suffers from long analysis times. Multicapillary gas chromatography microwave induced plasma optical emission spectrometry (MCGC-MIP-OES) combined with derivatization to alkyl compounds has been widely employed for speciation analysis of harmful organometallic pollutants Because of their toxicity and widespread distribution in environmental samples, butyltin and methylmercury compounds were most often determined among volatile organometallic species during the last 20 years. A method based on solid phase microextraction (SPME) in combination with MCGC separation and MIP-OES detection was developed and applied for ultra-trace mercury and tin speciation analysis in water samples. SPME is capable of interfacing with optical or mass spectrometry directly for detection of analytes without employing chromatographic separation [7,8] This arrangement provided fast desorption and high sample introduction efficiency, allowing determination of total content of the element of interest in a given sample. Two fiber coatings for headspace solid-phase microextraction (HS-SPME) are compared in terms of extraction efficiency
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