A. Buthe et E. Denker, QUALITATIVE AND QUANTITATIVE-DETERMINATION OF PCB CONGENERS BY USING A HT-5 GC COLUMN AND AN EFFICIENT QUADRUPOLE MS, Chemosphere, 30(4), 1995, pp. 753-771
The determination of CB congeners by means of a new HT-5 column (SGE A
ustralia) was carried out with a quadrupole GC-MS. A method is present
ed that permits the qualitative and quantitative determination of envi
ronmental and technical PCB mixtures with the help of only 14 single C
Bs, 2-4 reference CBs per degree of chlorination in SIM mode. More tha
n 70 individual CBs, including some coplanar congeners such as CB-77,
CB-126 and CB-169, were measured as pure standards. Additionally Cloph
en A30/A40/A60 and Aroclor 1254/1260 were measured. With our method a
total of 131 single CBs could be identified. For the quantitative dete
rmination several PCB congener groups were formed for each level of ch
lorination according to their fragmentation pattern. One CB with group
-typical fragmentation was used as reference for the calibration withi
n the group. The fragmentation pattern is strongly correlated with the
molecular structure of the single CB, so that CBs not available as pu
re standards can be identified. Some remarkable correlations between s
tructure of CBs of all degrees of chlorination and their fragmentation
in MS EI-mode were discovered. A similar retention time does not mean
a similar fragmentation pattern of these CBs and vice versa. The meas
urements were carried out in scan mode measuring masses 100-650 and in
SIM-mode, considering the [M](+), [M-CL](+) and [M-2Cl](+) ions.