Electron conductivity detector

The extraction of the AOT samples consisted of taking a 50-mL subsample and extracting by separatory funnel with hexane and 10% NaCl in water. The cleaned-up and dried hexane extract was then injected onto a gas chromatograph (GC) with an ECD (electron conductivity detector). The minimum quantifiable limit (MQL), or limit of quantification, for the method was 0.002 ug/mL dislodging solution. A typical set of chromatograms can be seen in Figures 1 and 2. 

The chromatogram can finally be used as the series of bands or zones of components or the components can be eluted successively and then detected by various means (e.g. thermal conductivity, flame ionization, electron capture detectors, or the bands can be examined chemically). If the detection is non-destructive, preparative scale chromatography can separate measurable and useful quantities of components. The final detection stage can be coupled to a mass spectrometer (GCMS) and to a computer for final identification. 

The detector. The function of the detector, which is situated at the exit of the separation column, is to sense and measure the small amounts of the separated components present in the carrier gas stream leaving the column. The output from the detector is fed to a recorder which produces a pen-trace called a chromatogram (Fig. 9.1fr). The choice of detector will depend on factors such as the concentration level to be measured and the nature of the separated components. The detectors most widely used in gas chromatography are the thermal conductivity, flame-ionisation and electron-capture detectors, and a brief description of these will be given. For more detailed descriptions of these and other detectors more specialised texts should be consulted.67 69... 

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. 

EC = electrical conductivity detector ECD = electron capture detector FPD = flame photometric detector GC = gas chromatography HPLC = high performance liquid chromatography NPD = nitrogen phosphorus detector TID = thermionic detector UV = ultraviolet spectroscopy... 

TEM observation and elemental analysis of the catalysts were performed by means of a transmission electron microscope (JEOL, JEM-201 OF) with energy dispersion spectrometer (EDS). The surface property of catalysts was analyzed by an X-ray photoelectron spectrometer (JEOL, JPS-90SX) using an A1 Ka radiation (1486.6 eV, 120 W). Carbon Is peak at binding energy of 284.6 eV due to adventitious carbon was used as an internal reference. Temperature programmed oxidation (TPO) with 5 vol.% 02/He was also performed on the catalyst after reaction, and the consumption of O2 was detected by thermal conductivity detector. The temperature was ramped at 10 K min to 1273 K. 

ECD = electron capture detector FID = flame ionization detection GC = gas chromatography HECD = Hall electrolytic conductivity detector HRGC = high-resolution gas chromatography HSD = halogen-specific detector H2SO4 = sulfuric acid MS = mass spectrometry NR = not reported PID = photoionization detection UV = ultraviolet detection... 

The product gases were continuously analyzed for NO and NO2 using a chemiluminescent analyzer, and discontinuously for N2O, N2, CO, CO2 and O2 by GC equipped with a thermal conductivity detector and an electron capture detector, specifically for the N2O analysis, using a Poraplot Q column and a molsieve 5A column for separation. 

Detectors range from the universal, but less sensitive, to the very sensitive but limited to a particular class of compounds. The thermal conductivity detector (TCD) is the least sensitive but responds to all classes of compounds. Another common detector is the flame ionization detector (FID), which is very sensitive but can only detect organic compounds. Another common and very sensitive detector is called electron capture. This detector is particularly sensitive to halogenated compounds, which can be particularly important when analyzing pollutants such as dichlorodiphenyltrichloroethane (DDT) and polychlorobiphenyl (PCB) compounds. Chapter 13 provides more specific information about chromatographic methods applied to soil analysis. 

There are four main types of detectors used in GC thermal conductivity detector (TCD), also called a hot wire detector, flame ionization detector (FID), electron capture detector (ECD), and quadruple mass spectrometer (MS)... 

Match the detector with the items that follow thermal conductivity detector, flame ionization detector, electron capture detector, and mass spectrometer detector. 

Of the thermal conductivity, flame ionization, and electron capture detectors, which... 

AOAC = Assocition of Official Analytical Chemists ASTM = American Society for Testing and Materials Cl = chemical ionization ECD = electron capture detection ELCD = electrolytic conductivity detector EPA = Environmental Protection Agency GC = gas chromatography GPC = gel permeation chromatography ... 

ECD = electron capture detection ELCD = electrolytic conductivity detector EPA = Environmental Protection Agency GC = gas... 

Infrared spectra were recorded on a Perkin Elmer Model 567 Spectrophotometer. Ultraviolet spectra were obtained on a Cary 1756 Spectrophotometer. Gas chromatograms were recorded on a Tracor Model 220 with electron capture detector. High pressure liquid chromatography studies were conducted with a Waters Model ALC-200 with ultraviolet and refractive index detectors. 

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... 

ECO = electron capture detector ED = electrochemical detector FID st flame ionization detector GC = gas chromatography HECD = Hall s electrolytic conductivity detector HPLC = high performance liquid chromatography MEC = molecular emission cavity analysis MS - mass spectrometry HD = photo-ionization detector... 

Two types of conductivity detectors exist the contact conductivity detector, where the electrodes are in direct contact with the electrolyte, and the contactless coupled conductivity detector (C D also called oscillometric detector). With this detector, two stainless-steel tubes that act as electrodes are mounted on a capillary at a certain distance from each other. By applying an oscillation frequency, a capacitive transition occurs between the actuator electrode and the liquid inside the capillary. After having passed the detection gap between the electrodes, a second capacitive transition between the electrolyte and the pickup electrode occurs (see Figures 7 and 8 which is an example of separation of cations). In different reviews, Zemann and Kuban and Hauser discuss the advantages of this technique which include rather simple mechanical parts and electronics, and Kuban et al. compared several C D detectors. This technique has also been used as a detector for analysis by microchip CE. C" D detectors are available to be mounted on existing CE instruments. 

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