A new instrumental method for the characterization of the analyte 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) by selected reaction monitoring (SRM) analysis is investigated. The method uses high-resolution gas chromatography coupled to a hybrid tandem mass spectrometer. The technique was evaluated with regard to four performance parameters: sensitivity, linearity, repeatability and selectivity. The method compares favorably with the traditional selected ion monitoring HRGC/HRMS technique, and the selectivity of the new method is shown to surpass the established HRGC/HRMS method. This new method could allow the characterization of samples that have undergone less rigorous cleanup than is now possible by the traditional mass spectrometric methods. The presence of TCDDs in a real sample was confirmed by using the new HRGC/(hybrid)MS/MS SRM method, which was not possible by using HRGC/HRMS analysis.

Environmental sample extracts contain a variety of volatile and nonvolatile organic compounds exhibiting a range of polarities and concentrations. Although gas chromatography/mass spectrometry (GC/MS) is the method of choice thus far for such analyses, this technique used alone cannot adequately characterize the volatiles in such samples and is not amenable to environmental nonvolatiles. A more complete characterization of environmental and hazardous waste samples is required to assess the dangers posed to the nation's groundwater by hazardous waste dumps. Online spectral confirmation by directly linked GC/Fourier transform infrared (FTIR)/MS is shown to provide useful structural information on environmental volatiles in hazardous wastes, even when the analyte's spectrum is not in either spectral database. This information can lead to biological-hazard estimation. The diffuse reflectance Fourier transform infrared (DRIFT) technique, used in conjunction with thermospray MS or fast atom bombardment (FAB) MS, provides confirmed identifications or confirmed compound class assignments of organic nonvolatiles in solid wastes. This is believed to be the first report of spectral confirmation (identification or functionality) of organic volatiles and nonvolatiles in environmental samples.