Instrumentation capillary column

This overview concerns the new chromatographic method - capillary electrochromatography (CEC) - that is recently receiving remarkable attention. The principles of this method based on a combination of electroosmotic flow and analyte-stationary phase interactions, CEC instrumentation, capillary column technology, separation conditions, and examples of a variety of applications are discussed in detail. 

Capillary Columns. Capillary columns have no packing the liquid phase is simply applied directly to the walls of the column. These columns are referred to as waU-coated, open-tubular (WCOT) columns. The reduction in surface area (compared to packed columns) is compensated for by tiny column diameters (perhaps 0.1 mm) and impressive lengths (100 m is not uncommon). Capillary columns are the most powerful columns used for analytical separations. Mixtures of several hundred compounds can be completely resolved on a capillary GC column. These columns require a more sophisticated and expensive chromatography instrument. Capillary columns, because of their tiny diameters, can accommodate only very small samples, perhaps 0.1 jxL or less of a dilute solution. Capillary columns cannot be used for preparative separations. 

The most common mobile phases for GC are He, Ar, and N2, which have the advantage of being chemically inert toward both the sample and the stationary phase. The choice of which carrier gas to use is often determined by the instrument s detector. With packed columns the mobile-phase velocity is usually within the range of 25-150 mF/min, whereas flow rates for capillary columns are 1-25 mF/min. Actual flow rates are determined with a flow meter placed at the column outlet. 

Time, Cost, and Equipment Analysis time can vary from several minutes for samples containing only a few constituents to more than an hour for more complex samples. Preliminary sample preparation may substantially increase the analysis time. Instrumentation for gas chromatography ranges in price from inexpensive (a few thousand dollars) to expensive (more than 50,000). The more expensive models are equipped for capillary columns and include a variety of injection options and more sophisticated detectors, such as a mass spectrometer. Packed columns typically cost 50- 200, and the cost of a capillary column is typically 200- 1000. 

Although the OTHdC has several unique applications in polymer analysis, this technique has several limitations. First, it requires the instrumentation of capillary HPLC, especially the injector and detector, which is not as popular as packed column chromatography at this time. Second, as discussed previously, the separation range of a uniform capillary column is rather narrow. Third, it is difficult to couple capillary columns with different sizes together as SEC columns. 

The thermal sweeper is a commercial product licensed to Zoex Corporation, Lincoln, NA, USA (16). The sweeper incorporates a slotted heater (operated at about 100 °C above the oven temperature) which passes over the capillary column (normally an intermediate thicker film column is used in this region as an accumulator zone). Eigure 4.3 is a schematic diagram of how the instrumental arrangement may be considered. The greater temperature of the rotating sweeper forces the solute which has been retained in the phase in the accumulator section to be volatilized out of the phase into the carrier gas stream, and then bunched up and brought forward... 

SFC has been performed with either open capillary columns similar to those used in GC or packed columns transferred from LC, and the instrumentation requirements differ for these two approaches [12]. This chapter will focus on the use of packed column technology because of its dominance in the area of pharmaceutical compound separations. Current commercial instrumentation for packed column SFC utilizes many of the same components as traditional LC instruments, including pumps, injection valves, and detectors. In fact, most modem packed column SFC instm-ments can also be used to perform LC separations, and many of the same stationary phases can be used in both LC and SFC [9]. 

In chromatography-FTIR applications, in most instances, IR spectroscopy alone cannot provide unequivocal mixture-component identification. For this reason, chromatography-FTIR results are often combined with retention indices or mass-spectral analysis to improve structure assignments. In GC-FTIR instrumentation the capillary column terminates directly at the light-pipe entrance, and the flow is returned to the GC oven to allow in-line detection by FID or MS. Recently, a multihyphenated system consisting of a GC, combined with a cryostatic interfaced FT1R spectrometer and FID detector, and a mass spectrometer, has been described [197]. Obviously, GC-FTIR-MS is a versatile complex mixture analysis technique that can provide unequivocal and unambiguous compound identification [198,199]. Actually, on-line GC-IR, with... 

Valproic acid has been determined in human serum using capillary electrophoresis and indirect laser induced fluorescence detection [26], The extract is injected at 75 mbar for 0.05 min onto a capillary column (74.4 cm x 50 pm i.d., effective length 56.2 cm). The optimized buffer 2.5 mM borate/phosphate of pH 8.4 with 6 pL fluorescein to generate the background signal. Separation was carried out at 30 kV and indirect fluorescence detection was achieved at 488/529 nm. A linear calibration was found in the range 4.5 144 pg/mL (0 = 0.9947) and detection and quantitation limits were 0.9 and 3.0 pg/mL. Polonski et al. [27] described a capillary isotache-phoresis method for sodium valproate in blood. The sample was injected into a column of an EKI 02 instrument for separation. The instrument incorporated a conductimetric detector. The mobile phase was 0.01 M histidine containing 0.1% methylhydroxycellulose at pH 5.5. The detection limit was 2 pg/mL. 

Noncondensable gases leaving the condensation vessels were depressurized (by means of an electronic back-pressure, Brooks Instrument model 5866), totalized (by means of an on-line flow gas meter, Ritter model TG05-5), and periodically analyzed with an on-line GC (Hewlett-Packard model 6890) equipped with three columns and two detectors for the analysis of Cj-C10 hydrocarbons (A1203 plot capillary column connected to a flame ionization detector), H2, CH4,... 

Capillary Breakup Extensional Rheometer (CaBER), 21 740 Capillary columns, 6 377, 408 band broadening, 6 412 instrumentation, 6 424 speciality appbcations, 6 427t Capillary condensation, 1 585, 591 ... 

The best-known and the most commonly used hyphenated method is GC-MS more specifically, and most commonly, capillary column GC combined with quadrupole MS. This type of instrumentation is controlled by computer and data collected and analyzed by dedicated computer programs. The mass spectra produced by the analytes can be compared to those in a library of mass spectra of known compounds using a computer search algorithm. The computer program finds known compounds that best match the spectra of the analytes of interest. 

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