A robust analytical method is presented for the direct determination of polychlorinated biphenyls in soil samples by thermal desorption/gas chromatography/ mass spectrometry. The method is simple to perform (thermal desorption and analysis are performed in-line employing a limited amount of sample, 2 mg) and eliminates the need for any solvent and time-consuming extraction. The analytical procedure was optimized using a soil sample spiked with Aroclor 1254 and Aroclor 1260 and validated with a certified industrial soil sample for which the concentration of thirteen PCB congeners are known. Limits of detection were sensitive to matrix effects and varied substantially among analytes. The matrix effect resulted in a reduction of the limits of detection by 1.5-10 times. However, it was found that the matrix effect is not due to ion suppression but to the increase of the noise of selected ion monitoring (SIM) traces, indicating that no limitation exists with using a single surrogate standard. By employing a 13C-labelled PCB internal standard, limits of detection in the range of 0.8 to 10 mgg1 of soil were obtained. The obtained experimental results demonstrated that the proposed analytical method can be conveniently applied for screening a large number of heavily contaminated soil samples thus avoiding the employment of harmful solvents and time-consuming extraction procedures.
Direct analysis of polychlorinated biphenyls in heavily contaminated soils by thermal desorption/gas chromatography/mass spectrometry
Mascolo G;Bagnuolo G;Uricchio V
2013
Abstract
A robust analytical method is presented for the direct determination of polychlorinated biphenyls in soil samples by thermal desorption/gas chromatography/ mass spectrometry. The method is simple to perform (thermal desorption and analysis are performed in-line employing a limited amount of sample, 2 mg) and eliminates the need for any solvent and time-consuming extraction. The analytical procedure was optimized using a soil sample spiked with Aroclor 1254 and Aroclor 1260 and validated with a certified industrial soil sample for which the concentration of thirteen PCB congeners are known. Limits of detection were sensitive to matrix effects and varied substantially among analytes. The matrix effect resulted in a reduction of the limits of detection by 1.5-10 times. However, it was found that the matrix effect is not due to ion suppression but to the increase of the noise of selected ion monitoring (SIM) traces, indicating that no limitation exists with using a single surrogate standard. By employing a 13C-labelled PCB internal standard, limits of detection in the range of 0.8 to 10 mgg1 of soil were obtained. The obtained experimental results demonstrated that the proposed analytical method can be conveniently applied for screening a large number of heavily contaminated soil samples thus avoiding the employment of harmful solvents and time-consuming extraction procedures.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
