Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

Abstract

SummaryA method is proposed for the extraction and determination of organomercury compounds and Hg(ll) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in sphtless mode.Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables:sample volume, NaBPh4 volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirabilily function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species.

Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry

“…Considering the high toxicity of mercury and its wide distribution in the biosphere, analytical procedures providing high sensitivity for the determination of this pollutant have been developed. Studies performed on the determination of mercury using SPME for preconcentration generally have relied on fibers such as polydimethylsiloxane [33][34][35][36][37][38][39], polydimethylsiloxane/divinylbenzene [33] or carboxen/polydimethylsiloxane [39].…”

Application of Solid-Phase Microextraction Combined with Derivatization for Polar Compound Sampling in Environmental Analysis

“…HS-SPME technique is widely used for extracting various kinds of chemicals. Among them, in-vial (in situ) derivatization is frequently used for haloacetic acids (HAAs) [21,23] and acetic acid [67], aldehyde compounds [25,124,165], phenoxy acid herbicides [68], phenolic pollutants [17,18,82,91,159], aliphatic amines [120,125], acaricide fenbutatin oxide (FBTO) [131], acetone [111], selective serotonin reuptake inhibitors (SSRIs) such as venlafaxine, fluvoxamine, fluoxetine, citalopram, and sertraline [97], and organometallic compounds such as organotin [29,31,86,87,127,128,138,139,160], organolead [31,86,89,160], and organomercury [31,128,129,140,160]. On-fiber in situ derivatization is used for analyzing chemicals such as aldehyde compounds [27,105,164], carbonyls compounds [28], and thiol compounds [171].…”

Applications of solid phase microextraction for the determination of metallic and organometallic species

“…Carro et al [48] proposed a method for the speciation of mercury compounds by SPME-GC-MIP-AES in seawater samples. The Hg species were derivatized with Na tetraphenylborate, sorbed on a PDMS-coated fused-silica fiber, and desorbed in the injection port of the GC in splitless mode.…”