Synthesis, isolation and purification of C 10–C 13 polychloro- n-alkanes for use as standards in environmental analysis

Abstract

Short chain (C 10–C 13) polychloro- n-alkanes ( sPCAs) mixtures were synthesized by refluxing pure n-alkane (>99%) with sulfuryl chloride (SO 2Cl 2) in the presence of UV-light (550 W). The free radical initiated reactions produced analogs containing ∼4–9 chlorine atoms on each carbon chain. Purification of reaction products was achieved by adsorption chromatography on Florisil. The products were characterized by high-resolution gas chromatography/mass spectrometry (HRGC/MS) operated in the electron capture negative ionization (ECNI) and in electron ionization (EI) modes. Individual standards can now be combined to create standards whose profiles resemble that of environmental samples. Quantification of a known amount of the newly synthesized sPCAs mixture, using an industrial formulation as an external standard, resulted in an overestimation (∼28%) in its true value.