Conductivity detectors, capillary

Bioluminescence detector Charge-coupled device Contactless-conductivity detector Capillary electrophoresis Capillary electrophoresis-Electrochemistry Collision-induced dissociation Chemiluminescence detector Sodium chlorate-nitrobenzene Commercial off-the-shelf (U.S. Army) Cold Regions Research and Development Center Croatian Mine Action Center Council of Scientific and Industrial Research,... 

Figure 4 Eiectropherogram of the anaiysis of cationic impurities in drug Carbetocin with conductivity detector. Capillary, 70.0cm, 50pm, fused silica running electrolyte, SOmmoll" histidine, 30 mmol 1 2-morpholinoethan-sulfonic acid separation voltage, 30 kV injection, hydrodynamic, 20mbarfor6s detection, conductometric. Peaks 1, K" 2, Ba 3, Ca + 4, Mg " 5, Na" 6, Li". (Kindly provided by Dr. I. Jelfnekfrom our Department.)...

Zhou and colleagues determined the %w/w H2O in methanol by GG, using a capillary column coated with a nonpolar stationary phase and a thermal conductivity detector. A series of calibration standards gave the following results. 

Limits of detection become a problem in capillary electrophoresis because the amounts of analyte that can be loaded into a capillary are extremely small. In a 20 p.m capillary, for example, there is 0.03 P-L/cm capillary length. This is 1/100 to 1/1000 of the volume typically loaded onto polyacrylamide or agarose gels. For trace analysis, a very small number of molecules may actually exist in the capillary after loading. To detect these small amounts of components, some on-line detectors have been developed which use conductivity, laser Doppler effects, or narrowly focused lasers (qv) to detect either absorbance or duorescence (47,48). The conductivity detector claims detection limits down to lO molecules. The laser absorbance detector has been used to measure some of the components in a single human cell (see Trace AND RESIDUE ANALYSIS). 

In the 1970s a new analysis method was developed, referred to as isota-chophoresis [247]. Capillary isotachophoresis with conductivity detector is very useful in detergent analysis for the determination of all kinds of ionic species [248]. It is also useful for the determination of MCA in ether carboxylates. 

The gas chromatograph is better to be equipped both with a thermal conductivity detector (TCD) and with a flame ionization detector (FID). The latter is extremely useful in the analysis of organic substances at low concentrations. Packed columns are normally used, although capillary columns offer certain advantages in the analysis of a variety of products. Some of the major companies that supply gas chromatographs are ... 

The catalytic reforming of CH4 by CO2 was carried out in a conventional fixed bed reactor system. Flow rates of reactants were controlled by mass flow controllers [Bronkhorst HI-TEC Co.]. The reactor, with an inner diameter of 0.007 m, was heated in an electric furnace. The reaction temperatoe was controlled by a PID temperature controller and was monitored by a separated thermocouple placed in the catalyst bed. The effluent gases were analyzed by an online GC [Hewlett Packard Co., HP-6890 Series II] equipped with a thermal conductivity detector (TCD) and carbosphere column (0.0032 m O.D. and 2.5 m length, 80/100 meshes), and identified by a GC/MS [Hewlett Packard Co., 5890/5971] equipped with an HP-1 capillary column (0.0002 m O.D. and 50 m length). 

The thermal conductivity detector (TCD) is a classical detector for both packed and capillary columns. A schematic representation of a modern... 

Fig. 14.6. Schematic diagram of a capillary thermal conductivity detector showing both the reference and analytical flows. Reprinted with permission from the 6890 Gas Chromatograph Operating Manual. Copyright (2004), Agilent Technologies.

J. Muzikar, T. van de Goor, B. Gas and E. Kenndler, Extension of the application range of UV-absorbing organic solvents in capillary electrophoresis by the use of a contactless conductivity detector. J. Chromatogr.A 924 (2001) 147-154. 

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. 

Kuban, P., and Hauser, P. C. (2005). Application of an external contactless conductivity detector for the analysis of beverages by microchip capillary electrophoresis. Electrophoresis 26, 3169—3178. 

Ho JSY. 1989. A sequential analysis for volatile organics in water by purge-and-trap capillary column gas chromatography with photoionization and electrical conductivity detectors in series. J Chromatogr Sci 27 91-98. 

CZE = capillary zone electrophoresis EC = electrochemical detector GC = gas chromatography HCD = Hall conductivity detector HPLC = high performance liquid chromatography IDMS = isotope dilution mass spectrometry MS = mass spectrometry RSD = relative standard deviation SEE = supercritical fluid extraction SPE = solid phase extraction UV = ultraviolet absorbance detection... 

Wang, J., G. Chen, and A. Muck, Jr. Movable contactless conductivity detector for microchip capillary electrophoresis. Anal. Chem. 75, 4475-4479 (2003). 

Hydrogen gas may be analyzed by GC using a thermal conductivity detector (TCD). A molecular sieve 5A capillary column and helium as the carrier gas should be suitable for analysis. A common method of analyzing hydrogen involves combustion with oxygen to produce water, which is trapped on an adsorbent and determined by gravimetry. 

Other electrode configurations, such as the radial arrangement consisting of four thin wires placed perpendicularly around the circumference of the separation capillary column, have found less application due to more complicated construction and restriction in space and diameter of the separation capillary [56]. Due to its low cost, robustness, minimal maintenance demands, possibility to be freely moved along the capillary [57], or combined with either UV-absorbance [58] or fluorescence [59] detection, the capacitively coupled contactless conductivity detector has recently gained wide acceptance not only for the determination of inorganic ions but also for biomolecules and organic ions, as it has been recently comprehensively reviewed by Kuban and Hauser [1]. 

The measurement electrodes can be wrapped around, threaded onto, or painted over a standard capillary. The use of a grounded shield in between the measurement electrodes greatly reduces stray capacitance. (B) Simplified circuit diagram for a contactless conductivity detector. includes double layer capacitance Cjj as well as the capacitance across the capillary wall. 

Fanali et al. have described a capillary isotachophoresis method for the determination of procaine in pharmaceuticals [ 150]. The drug was determined in a 6 pL sample of solution (Spofa product, obtained from Czechoslovakia, and diluted 180-fold) by cationic isotachophoresis in the single column mode. The system used a PTFE capillary column (20 cm x 0.3 mm) and a conductivity detector. The separation was carried out at room temperature, at 50 pA (but switched to 25 pA during detection). 

TPR of the samples in flowing He or H2 were performed in a Pyrex flow system which was also used for catalytic reactions. Acid properties of the samples were probed by TPD of NH3 preadsorbed at RT. The analysis of gaseous products was made by an on-line mass spectrometer or a thermal conductivity detector. Reactions of n-hexane in the presence of excess H2 were carried out at 623 K and atmospheric pressure. A saturator immersed in a constant temperature bath at 273 K was used to produce a reacting mixture of 6% n-hexane in H2. Reaction products were analyzed by an online gas chromatograph (HP-5890A) equipped with a flame ionization detector and an AT-1 (Alltech) capillary column. 

P. Kuban and P.C. Hauser, Effects of the cell geometry and operating parameters on the performance of an external contactless conductivity detector for microchip electrophoresis, Lab Chip, 5 (2005) 407-415. J.G.A. Brito-Neto, J.A.F. da Silva, L. Blanes and C.L. do Lago, Understanding capacitively coupled contactless conductivity detection in capillary and microchip electrophoresis. Part 2. Peak shape, stray capacitance, noise, and actual electronics, Electroanalysis, 17 (2005) 1207-1214. 

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