Headspace Solid Phase Micro Extraction GC‐ECD Determination of Volatile Organic Chlorinated Hydrocarbons in Soils

Abstract

Soil samples were suspended in a suitable aqueous solvent and a solid phase microextraction (SPME) fibre was used to sample the headspace (HS) for five volatile chlorinated compounds (VOX). Their determination was made by GC-ECD technique in the splitless mode. Preliminary studies on the effects of methanol and of the sand/clay ratio on the fibre extraction were made. Four experimental factors, namely, extraction time, extraction temperature, pH and NaCl%, able to affect distribution of the analytes among the four different phases, were varied in suitable ranges. A multivariate approach applied to the face centred cube (FCC) experimental design, was used to try to optimise the overall sample response. The suitable set of factors found for the determination of chloroform, 1,2-dichloroethane, trichloroethylene, 1,1 ,2-trichloroethane, 1,1,2,2-tetrachloroethane, was a compromise among the relevant optimal factor sets of the single analytes. Detection limits of 0.003 ng, 0.022 ng, 0.001 ng, 0.015 ng and 0.002 ng were found respectively for the five cited analytes. The method was successfully used to determine the analyte contents in two real soils sampled in an industrial area.

Headspace solid-phase microextraction for the determination of volatile sulfur compounds in odorous hyper-eutrophic freshwater lakes using gas chromatography with flame photometric detection

“…VSCs, such as hydrogen sulfide (H 2 S), dimethyl sulfide (DMS), methanethiol (MeSH), dimethyl disulfide (DMDS), dimethyl trisulfide (DMTS), carbonyl sulfide (OCS), and carbon disulfide (CS 2 ), are released from natural sources, including oceans, marshes, soils, vegetation, and geothermal and volcanic activity, as well as from anthropogenic activities that involve biogas production, sewage treatment, landfilling, pulp milling, and slaughtering [4][5][6]. In modern society, eutrophication is a serious problem in freshwater lakes that are extensively used for not only agricultural, fishery and industrial purposes but also as sources of drinking water.…”

Trace level determination of trichloroethylene in biological samples by headspace solid‐phase microextraction gas chromatography/negative chemical ionization mass spectrometry

“…Solid phase microextraction (SPME) is a simple and efficient, solvent‐free sample preparation technique, suitable for both qualitative and quantitative analysis of volatile and semivolatile compounds in aqueous and solid matrices 1. SPME has been widely used for analyses in different fields, such as environmental monitoring, foods, flavors, fragrances, wines, biological fluids and breath analyses 2–11. Headspace (HS)‐SPME has been frequently used in biological monitoring, e.g.…”

Determination of trichloroethylene in biological samples by headspace solid-phase microextraction gas chromatography/mass spectrometry

“…Furthermore, headspace SPME methods can reduce matrix effects, because the biological macromolecules in the sample do not volatilize into the headspace. Several methods have been published describing the use of SPME for the analysis of TCE [23][24][25][26][27][28][29][30]. Some of these are focused on the determination of TCE in environmental media, such as air, drinking water and soil [23][24][25][26].…”