The Application of TD/GC/NICI–MS with an Al2O3-PLOT-S Column for the Determination of Perfluoroalkylcycloalkanes in the Atmosphere

Abstract

A modified method for the quantitative determination of atmospheric perfluoroalkylcycloalkanes (PFCs) using thermal desorption coupled with gas chromatography and detection by negative ion chemical ionization–mass spectrometry was developed. Using an optimized analytical system, a commercially available Al2O3 porous layer open tubular (PLOT) capillary column (30 m × 0.25 mm) deactivated with Na2SO4 was used for separation of PFCs. Improvements in the separation of PFCs, the corresponding identification and the limit of detection of PFCs using this method and column are presented. The method was successfully applied to determine the atmospheric background concentrations of a range of PFCs from a number of samples collected at a rural site in Germany. The results of this study suggest that the method outlined using the Al2O3-PLOT-S capillary column has good sensitivity and selectivity, and that it can be deployed in a routine laboratory process for the analysis of PFCs in the future research work. In addition, the ability of this column to separate the isomers of one of the lower boiling PFCs (perfluorodimethylcyclobutane) and its ability to resolve perfluoroethylcyclohexane offer the opportunity for single-column analysis for multiple PFCs.

An airborne perfluorocarbon tracer system and its first application for a Lagrangian experiment

“…The measured background concentrations of PMCP at the ground near Miri range between 5.18 and 8.95 fmol mol −1 , with a mean value of 6.62 fmol mol −1 and a standard deviation of 1.02 fmol mol −1 (6.62 ± 1.02 fmol mol −1 ). This is comparable to PMCP levels reported from previous field experiments (Kim et al, 2002;Simmonds et al, 2002;Watson et al, 2007;Ren et al, 2014). In the following subsections, the analytical results of the tracer measurements with PERTRAS are presented and comparisons between the measurement and HYS-PLIT simulation are discussed.…”

“…Here only a brief description of the analytical process is given. More details are given by Ren et al (2014). Thermal desorption was carried out with a thermal desorber ATD650 (PerkinElmer, USA).…”

“…Methane (N55 quality, Air Liquide) was used as reagent gas. The GC-MS interface and the source temperature were set to 190 • C. It has been demonstrated by Ren et al (2014) that this detection system can be used for routine laboratory analysis of several PFCs with good sensitivity and selectivity including PMCP, PMCH, PDCH, PDCB, and PECH (perfluoroethylcyclohexane).…”

Urban Pollutant Transport and Infiltration into Buildings Using Perfluorocarbon Tracers

“…Bag samples were analysed at the Bristol laboratory using an Agilent Gas chromatograph-mass spectrometer run in chemical ionization negative ion mode (NICI GC-MS, Agilent Technologies, Santa Clara, CA, USA). The GC was fitted with a 30 m × 0.25 mm × 5.0 μm Al2O3-PLOT-S capillary column (HP-PLOT Al 2 O 3 S, Agilent Technologies, Santa Clara, CA, USA) and used the temperature profile described in Ren et al [ 31 ]. The GC-MS was front-ended by a bespoke preconcentrator (adsorption, desorption system; ADS) [ 32 ] which pre-concentrated air samples onto a cryogenic trap.…”

“…From the ratio of peaks on the GC-MS, the two isomers of mPDMCH were quantified at 2.68 ppt of mc-PDMCH and 1.59 ppt of mt-PDMCH. In this analysis we concentrate on mc-PDMCH as mt-PDMCH co-elutes with pc-PDMCH on the current column [ 31 ]. The GC-MS response to standard concentration drifted less than 2% during the analysis.…”