Stir bar sorptive extraction for the analysis of short‐chain chlorinated paraffins in water

Abstract

Stir bar sorptive extraction for the analysis of shortchain chlorinated paraffins in water An optimised method using stir bar sorptive extraction (SBSE) and a thermal desorption-GC-electron capture detector (GC-ECD) for the determination of short-chain chlorinated paraffins from water samples was developed. Recoveries near to 100% were obtained by using 20 mm60.5 mm (length6film thickness) PDMS commercial stir bars from 200 mL spiked water samples and 20% methanol addition with an extraction period of 24 h. Method sensitivity, linearity and precision were evaluated for surface water and wastewater spiked samples. A LOD of 0.03 and 0.04 lg/L was calculated for surface and wastewater, respectively. The precision of the method given as an RSD was below 20% for both matrices. The developed method was applied for the analysis of two real samples from a contaminated river and a wastewater treatment plant. Results were in accordance with those obtained using a previously developed method based on solid phase microextraction (SPME).

Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

“…The low mobility of high molecular weight compounds in aqueous phase implies indeed a slow kinetic A c c e p t e d M a n u s c r i p t 18 mass transfer. Furthermore, Llorca-Porcel et al [23] determined an equilibrium time as long as 24 hours for SCCPs analysis by SBSE, which is consistent with the SPME equilibrium duration hereby found and the use of a thicker PDMS coating on the Twister ® .…”

“…replicates. A c c e p t e d M a n u s c r i p t 33 [19,21] SPE with GC/ECNI-MS [20] DI-SPME with GC/ECNI-MS [20] SBSE with GC/ECD [23] HS-SPME with GC/ECNI-MS (this work) 0.05 (seawater) a n.r. : not reported b : LOD obtained by using DI-SPME coupled to GC/ECD c n.m.: not measured Table 4: Occurrences and concentration levels (ng.L -1 ) of SCCPs in south France aquatic environment.…”

“…Currently there is a growing analytical trend towards the use of environmentally friendly extraction techniques. Following this trend, solvent-free extraction techniques such as solid phase micro-extraction (SPME) [22] and stir bar sorptive A c c e p t e d M a n u s c r i p t 7 extraction (SBSE) [23] were successfully applied to SCCPs determination in waters. To bring down detection limits, both preconcentration techniques were coupled to GC/ECD analysis, which proved to be more sensitive for SCCPs detection but less specific as compared to GC/ECNI-MS.…”

Routine Method for the Analysis of Short‐Chain Chlorinated Paraffins in Surface Water and Wastewater

“…However, few data are available about the presence of SCCPs in surface and wastewater. SCCPs have been detected in influents of wastewater treatment plants (WWTPs) at concentrations ranging from 0.22 to 4.7 μg L −1 , while in effluents of WWTPs their concentrations were lower, from the ng L −1 level to the low μg L −1 . Regarding river and lake water, SCCPs have been found at concentrations between 3.5 and 1.7 μg L −1 .…”

“…Regarding river and lake water, SCCPs have been found at concentrations between 3.5 and 1.7 μg L −1 . In Spain, these compounds have been found in the Llobregat River (Barcelona) at concentrations from 0.12 to 2.1 μg L −1 , generally in sampling sites close to industrial areas.…”