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A methodology to quantify dialkylmercury compounds using Headspace Solid Phase Microextraction (HS-SPME) and Gas Chromatography with Atomic Emission Detection (GC-AED) was developed. The parameters for Hg detection were optimized by factorial design and response surfaces. Univariate experiments were employed to determine the HS-SPME conditions; 75 &#956;m Carboxen / PDMS and 65 &#956;m PDMS / DVB were the best fibers. However, the former was excluded from further experiments due to extensive thermal degradation of analytes during desorption. The optimized procedure allowed detection of the analytes from aqueous samples with LOD of 1.7 ng L-1 and 0.2 ng L-1 for dimethyl- and diethylmercury, respectively. The analytical curves are linear in the range from 36 to 180 ng L-1 (Me2Hg) and 38 to 190 ng L-1 (Et2Hg), with LOQ of 38 ng L-1 (Me2Hg) and 29 ng L-1 (Et2Hg) and correlation coefficients of 0.998 for Me2Hg and 0.999 for Et2Hg.Foi desenvolvida uma metodologia para quantificar compostos dialquilmercúricos usando Microextração em Fase Sólida em Headspace (HS-SPME) e Cromatografia Gasosa com Detecção por Emissão Atômica (GC-AED). Os parâmetros para detecção de Hg foram otimizados usando planejamento fatorial e superfícies de resposta. Experimentos univariados foram empregados para determinar as condições de HS-SPME; as melhores fibras foram 75 &#956;m de Carboxen / PDMS e 65 &#956;m de PDMS / DVB. Porém, as primeiras foram descartadas pela extensa degradação térmica dos analitos na dessorção. O procedimento otimizado permite detectar os analitos em amostras aquosas com limite de detecção de 1,7 e 0,2 ng L-1 para dimetil- and dietilmercúrio, respectivamente. As curvas analíticas são lineares nas faixas de 36 a 180 ng L-1 (Me2Hg) e 38 a 190 ng L-1 (Et2Hg), com limite de quantificação de 38 ng L-1 (Me2Hg) e 29 ng L-1 (Et2Hg) e coeficientes de correlação de 0,998 para Me2Hg e 0,999 para Et2Hg

Isolation and quantification of dialkylmercury species by headspace solid phase microextraction and gas Chromatography with Atomic Emission detection