Application of Headspace Solid-Phase Microextraction for Determination of Chloro-Organic Compounds in Sewage Samples

Abstract

Solid phase microextraction (SPME) has been optimized and applied to the determination of the volatile halogenated compounds (VHCs) and semi-volatile halogenated compounds (SVHCs). Three types of SPME fiber coated with different stationary phases (PDMS–100 μm, CAR/PDMS-75 μm, PDMS/DVB–65 μm) were used to examine their extraction efficiencies for the compounds tested. Experimental parameters such as the selection of SPME coatings, extraction time, and addition of salts were studied. The carboxen-polydimethylsiloxane (CAR/PDMS) fiber appears to be the most suitable for the determination of VHCs. Analytical parameters such as linearity, limit of detection, and precision were also evaluated. Application of ECD detector for the determination of VHCs and SVHCs allows their determination on the low concentration level, ranging from 0.005 to 0.8 μg/L−1. The HS-SPME-GC/ECD procedure gave good analytical precision expressed as relative standard deviation (RSD) (ranged from 5.08% to 8.07%) for a concentration level of 5 μg/L−1 and good linearity (r2 > 0.98) in a wide calibration range. The applied HS-SPME-GC/ECD method was found to be a quick and effective technique for the determination of microtrace amounts of volatile and semi-volatile halogenated compounds in samples containing high amounts of various organic compounds.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection

“…Literature headspace methods, both dynamic and static, generally involve the addition of a salt before agitation/heating to increase volatilisation of the target analytes [ 20 ]. To test the effect of salt addition, spiked standards were analysed after the addition and dissolution of salt (sodium sulphate) at varying masses, (dissolved masses of up to 2 g were tested).…”

“…The major interference in the case of THMs is that of haloacetic acids and haloacetonitriles, both of which have been shown to break down into THMs [ 4 ], providing false readings of both groups. In the present study, the volatilisation of other DBPs was eliminated by using a lower temperature and reduced agitation time and salt concentration than typical headspace methods [ 20 , 21 ]. This also allowed a much shorter analysis time of 10 min compared to the 20–30 min runtimes that are common for the analysis of multiple DBPs.…”

Characterization of volatile compounds in Cowart muscadine grape (Vitis rotundifolia) during ripening stages using GC-MS combined with principal component analysis

“…However, the use of solvent extraction methods has some disadvantages, such as possible sample contamination, an environmental burden, and loss of the VOCs owing to their degradation during the concentration step (4). In comparison, SPME is considered a more desirable technique for many flavor analyses because it is a rapid, inexpensive, and solvent-free technique that combines the extraction and concentration steps in the headspace (15). Thus, SPME has been widely used in many liquid and fragrance analyses.…”

Single Molecule Studies of Solvent-Dependent Diffusion and Entrapment in Poly(dimethylsiloxane) Thin Films

“…The ability of PDMS to absorb organics is also utilized in solid phase micro extraction fibers . In these applications, a thin coating of PDMS is cast onto a fiber, which is placed inside a syringe and subsequently used to remove a fraction of absorbable content from the headspace of a solution, or from the solution itself . The fiber can then be placed into the injection port of a gas chromatograph and heated to remove the absorbed content, thus resulting in a preconcentrated injection from which a quantitative analysis can be performed.…”