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

Short chain (C-10-C-13) polychloro-n-alkanes (sPCAs) mixtures were synthesi zed by refluxing pure n-alkane (>99%) with sulfuryl chloride (SO2Cl2) in th e presence of UV-light (550 W). The free radical initiated reactions produc ed analogs containing similar to 4-9 chlorine atoms on each carbon chain. P urification of reaction products was achieved by adsorption chromatography on Florisil. The products were characterized by high-resolution gas chromat ography/mass spectrometry (HRGC/MS) operated in the electron capture negati ve ionization (ECNI) and in electron ionization (EI) modes. Individual stan dards can now be combined to create standards whose profiles resemble that of environmental samples. Quantification of a known amount of the newly syn thesized sPCAs mixture, using an industrial formulation as an external stan dard, resulted in an overestimation (similar to 28%) in its true value. (C) 2000 Elsevier Science Ltd. All rights reserved.