Gt. Tomy et al., Synthesis, isolation and purification of C-10-C-13 polychloro-n-alkanes for use as standards in environmental analysis, CHEMOSPHERE, 40(6), 2000, pp. 679-683
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)
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