Synthesis and characterization of eight single chain length chlorinated paraffin standards and their use for quantification.

RATIONALE: Quantification of chlorinated paraffins (CPs) via gas chromatography coupled with electron capture negative ionization low-resolution mass spectrometry (GC/ECNI-MS) is a very common practice, although the quality of the results has been disputed due to insufficient mass resolution and the strong impact of the degree of chlorination on the GC/ECNI-MS response.
METHODS: For further tests we synthesized eight single chain length CP standards (C10 -C17 ) with chlorine contents between 51.1% and 61.3%. The individual single chain length standards, 1 + 1 mixtures of two chain length standards and self-prepared mixtures of short-chain and medium-chain CPs were quantified by linear regression according to a previously reported method (method 1) as well as by exponential regression (method 2).
RESULTS: Concentrations obtained from single chain length CP standards deviated between -74% and 152% from the target value. However, the error became smaller when self-prepared CP mixes with two and four chain lengths were analysed. For short-chain CP (SCCP) mixture analysis, both methods produced good results (<25% deviation from the target value). In the case of medium-chain CP (MCCP) mixtures, however, method 2 (17-34% deviation) was more accurate than method 1 (43-52% deviation).
CONCLUSIONS: Both methods 1 and 2 are fit for GC/ECNI-MS analysis of SCCP mixtures, while the improved method 2 is recommended for quantification of MCCP mixtures.