Analysis of short-chain chlorinated paraffins: a discussion paper

Pellizzato, Francesca; Ricci, Marina; Held, Andrea; Emons, Hendrik

doi:10.1039/b710053a

Cited by 32 publications

(17 citation statements)

References 33 publications

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“…Concentrations based solely on LRMS could even vary by up to 2 orders of magnitude (Pellizzato et al, 2007). Since 2010, five SCCPs ILSs were conducted, of which two were coordinated by Quality Assurance of Information for Marine Environmental Monitoring in Europe (QUASIMEME).…”

Section: Interlaboratory Studiesmentioning

confidence: 99%

Recent developments in capabilities for analysing chlorinated paraffins in environmental matrices: A review

et al. 2015

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Section: Interlaboratory Studiesmentioning

confidence: 99%

Recent developments in capabilities for analysing chlorinated paraffins in environmental matrices: A review

et al. 2015

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“…GC leads to better sensitivity, but interfering substances have to be eliminated before instrumental analysis. It is possible to quantify SCCPs, independent of the chlorine content, by the detection of the carbon skeleton [19] after catalytic removal of the chlorine within the injector of the gas chromatograph, followed by GC and detection by FID or MS. Using this technique analysis of the C-number distribution of SCCPs can be performed.…”

Section: Introductionmentioning

confidence: 99%

Determination of the Sum of Short Chain Polychlorinated n‐Alkanes with a Chlorine Content of Between 49 and 67% in Water by GC‐ECNI‐MS and Quantification by Multiple Linear Regression

Geiß¹,

Einax²,

Scott³

2010

CLEAN Soil Air Water

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This new approach for the quantification of the sum of short chain polychlorinated alkanes in mixtures (commonly abbreviated as SCCPs, where P stands for paraffin) with average chlorine contents between 49 and 67% and different C-number distributions is the background for ISO CD 12010, allowing standardized analysis according to the European water framework directive in unfiltered surface water, ground water, drinking water and waste water. A quantification method for the sum of short chain polychlorinated n-alkanes by GC-ECNI-MS (gas chromatography coupled with electron capture chemical ionization mass spectrometry), independent of the chlorine content and robust against changes in C-number distribution, was developed. This means that the very different response factors in GC-ECNI-MS, depending on the chlorine content, are no longer a problem for the analysis of SCCPs. Furthermore, problems with the selection of analytical standards due to batch dependent technical mixtures and different environmentally occurring mixtures can be overcome by using this robust method. The calibration was performed using synthetic mixtures mimicking a variety of different technically produced SCCP mixtures with average chlorine contents between 49 and 67% and different C-number distributions. By this means, the calibration is also traceable. The method was based on the integration of selected m/z value (mass/charge relation value) signals over the full retention range of the compounds. Quantification was performed using multiple linear regression calibration with two selected m/z signals, and verified with two other mass combinations. The selection of the m/z values used for quantification was carried out by means of an orthogonal calibration design. A stepwise procedure was utilized to produce the best quantification results, with the minimum number of quantification m/z signals, together with the minimization of potential interferences to be encountered in water analysis. The weighted sum of the peak areas of two m/z values, m/z 327 and 423, led to a sum determination which was applicable to the different SCCP mixtures most likely to be found in the aquatic environment. The problem with the very different response factors of the selected m/z values in GC-ECNI-MS, caused by the differing chlorine content of the SCCP mixtures, was overcome as well by forming the weighted sum of the two selected peak areas. The method was especially suitable for water analysis because of the low detection limit achieved by GC-ECNI-MS for chlorinated compounds.

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“…Most of the methods used for the determination of CPs are based on GC with electron capture detection (GC-ECD), or GC coupled to high or low resolution electron capture negative ion MS [12 -15]. As was explained by Pellizzato et al [16], the most recommended detection method for SCCPs are ECD or ECNI-MS. One of the difficulties encountered in the detection of SCCPs by MS electron impact (EI) is due to the large amount of fragmentation of these compounds, leading to the production of highly complex mixtures. For this reason, to realise detection at very low levels, detectors specifically for halogenated compounds (ECD) are required, or alternatively, the use of MS with lower fragmentation at the ionisation stage, as in the case of nega-tive chemical ionisation (ENCI-MS).…”

Section: Introductionmentioning

confidence: 99%

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

Llorca-Pórcel¹,

Martínez-Soriano²,

Valor³

2009

J of Separation Science

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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).

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Analysis of short-chain chlorinated paraffins: a discussion paper

Cited by 32 publications

References 33 publications

Recent developments in capabilities for analysing chlorinated paraffins in environmental matrices: A review

Recent developments in capabilities for analysing chlorinated paraffins in environmental matrices: A review

Determination of the Sum of Short Chain Polychlorinated n‐Alkanes with a Chlorine Content of Between 49 and 67% in Water by GC‐ECNI‐MS and Quantification by Multiple Linear Regression

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

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