VALIDATION OF AN IMPROVED EUROPEAN STANDARD METHOD FOR THE DETERMINATION OF PCBs IN OIL SAMPLES

Two European standard methods (EN 12766 and EN 61619) are currently used for the determination of PCBs in specific oil matrix. However, apolar matrix compounds (e.g. hydrocarbons) elute from the adsorbent together with the PCBs and are injected into the analytical system where their presence contaminates the inlet, detectors and columns; and decreases system performances. Insufficient cleanup causes delay of elution of PCBs from GC columns. By using new sulfoxide-bonded silica, PCBs are better separated from aliphatic hydrocarbons because the specificity of the stationary phase for these compounds is much higher that that used in both standard methods. A gas chromatograph AT6890 with two capillary columns of different polarities (HP-5MS and DB-1701) coupled to two μECDs is used. Oven temperature program is as followed: 90°C (1 min), 70°C/min to 180°C, 5°C/min to 230°C (0.1 min), 1.5°C/min to 280°C. Run time is 46 min. The procedure was validated through regular analysis of blanks, fortified samples (transformer oil, motor used and unused oil) and certified materials (BCR-449 and BCR-420, waste mineral oils, high and low PCB levels). Two internal standards were used (PCB 30 and PCB 209). An average recovery ± RSD of 82.8 ± 5.4 % was achieved for all six PCBs in different matrices. The LOQ per single PCB congener is 0.2 mg kg. The average recovery ± RSD for the BCR-420 is 92.0 ± 4.6 % and for the BCR-449 is 105 ± 2.5 % for all certified PCBs in waste oils.