ECD Characteristics

Discharge electrode Discharge corona Dopant inlet 

Nitrogen or hydrogen for pulsed mode operation 10% methane 

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ECD Characteristics. Compound-specific destructive concentration or mass-flow detector depending on operation compound sensitivities differ over a wide range useable primarily with isocratic RP-HPLC including some buffer salts, pre- or postcolumn derivatization can be used to increase number of measurable compounds. 

Ionisation detectors. An important characteristic of the common carrier gases is that they behave as perfect insulators at normal temperatures and pressures. The increased conductivity due to the presence of a few charged molecules in the effluent from the column thus provides the high sensitivity which is a feature of the ionisation based detectors. Ionisation detectors in current use include the flame ionisation detector (FID), thermionic ionisation detector (TID), photoionisation detector (PID) and electron capture detector (ECD) each, of course, employing a different method to generate an ion current. The two most widely used ionisation detectors are, however, the FID and ECD and these are described below. 

Electron transfer dissociation (ETD) is an ECD-like method with most of the same characteristics [21]. Like ECD, ETD yields abundant peptide backbone c- and z-type ions while often retaining such labile groups as peptide O/TV-glycosylation and phosphorylation [22]. Unlike ECD, ETD can be performed in the presence of an RF field. Here, anions created in a chemical ionization (Cl) source (see Section 2.1.7) are used as electron donors but the fragmentation pathways are essentially the same as for ECD. Commercial linear QIT instruments have recently become available with the ETD option. 

The best sensitivity for 1,2-dibromoethane quantification is obtained by either electron capture detector (ECD) or Hall electrolytic conductivity detector (HECD) in the halide detection mode, since these detectors are relatively insensitive to nonhalogenated species and very sensitive to halogenated species. Another common detection device is a mass spectrometer (MS) connected to a GC. The GC/MS combination provides unequivocal identification of 1,2-dibromoethane in samples containing multiple components having similar GC elution characteristics (see Table 6-2). To date, GC equipped with either ECD or HECD has provided the greatest sensitivity for detecting... 

Elemental composition C 7.81%, Cl 92.19%. Carhon tetrachloride may be analyzed by GC or GC/MS. For GC determination, an FID or a halogen-specific detector such as ECD or HECD may he used. Trace concentrations in aqueous matrix or soil, sediments or sohd wastes may he determined by purge and trap or thermal desorption techniques followed hy GC or GC/MS measurements. The characteristic masses for identification of CCI4 by GC/MS are 117, 119 and 121. 

Stabilization of a P-hairpin structure can be achieved in two ways, promoting a stable (or restricted) turn structure (as done with mimetics) or linking the two arms either chemically, or, more naturally, by hydrophobic interactions. In an approach to utilizing both methods, a D-Pro-Gly linkage was used to stabilize a left-handed turn (type I or II ) and various charged and hydrophobic residues were used to stabilize the molecule and enhance the interaction between arms. I252"254 Examples of these peptides studied in nonaqueous solution by IR, VCD and NMR spectroscopy exhibit characteristics of well-formed hairpins. 255 Alternatively, in aqueous solution, IR, VCD, and ECD results for related peptides agree with the NMR interpretation of conformations characterized as hairpins stabilized at the turn and frayed at the ends. 256 These latter results also have a qualitative match with theoretical simulations. Recently, examples of hydrophobically stabilized hairpins studied by NMR spectroscopy have avoided use of a nonnatural amino acid. 257,258 ... 

The confirmation of pesticides by GC/MS should be more reliable than that on the GC-ECD using an alternate column. Presence of stray interference peaks, even after sample cleanup, and the retention time shift and coelution problem, often necessitate the use of GC/MS in compounds identification If a quantitative estimation is to be performed, select the primary ion or one of the major characteristic ions of the compounds and compare the area response of this ion to that in the calibration standard. Quantitation, however, is generally done from the GC-ECD analysis, because ECD exhibits a much greater sensitivity than the mass selective detector (MSD). For example, while ECD is sensitive to 0.01 ng dieldrin, the lowest MSD detection for the same compound is in the range of 1 ng. The primary and secondary characteristic ions for qualitative identification and quantitation are presented in Table 2.20.3. The data presented are obtained under MS conditions utilizing 70 V (nominal) electron energy under electron impact ionization mode. 

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