Column, capillary velocity

Packed bed columns for CEO can also be obtained by using centripetal forces [49,141], Packing of the particles is obtained by centripetal acceleration through the capillary column. The velocity of the particles is given by the sedimentation velocity (used) as follows [49] ... 

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. 

Figure 5 shows that using average velocity data the extracted value for the multi-path term is negative, which is physically impossible, and, furthermore, for a capillary column should be zero or close to zero. In contrast, the extracted values for the different dispersion processes obtained from data involving the exit velocity give small positive, but realistic values for the multi-path term. 

The flow profiles of electrodriven and pressure driven separations are illustrated in Figure 9.2. Electroosmotic flow, since it originates near the capillary walls, is characterized by a flat flow profile. A laminar profile is observed in pressure-driven systems. In pressure-driven flow systems, the highest velocities are reached in the center of the flow channels, while the lowest velocities are attained near the column walls. Since a zone of analyte-distributing events across the flow conduit has different velocities across a laminar profile, band broadening results as the analyte zone is transferred through the conduit. The flat electroosmotic flow profile created in electrodriven separations is a principal advantage of capillary electrophoretic techniques and results in extremely efficient separations. 

Always adjust the carrier gas linear velocity to 20-40 cm/sec before heating the capillary column. Neglecting to supply carrier gas while heating a capillary column will destroy it. Avoid injecting samples containing inor-... 

Thus, the velocity oscillations, in the flow of an incompressible fluid, depend only on time, i.e., the liquid and vapor columns move in the capillary tube, on the whole, similar to a solid body. Bearing this in mind, we present the solution of Eq. (11.15) as follows ... 

Figure 2.7 Activity test of an uncoated fused silica capillary after deactivation with poly(phenyliaethylhydrosiloxane), (A), and before deactivation, (B). Precolunn 15 x 0.20 m I.D. coated with SE-54. Test columns 10 a x 0.20 I.D. The column tandem was programmed from 40 to I80 c at a C/min after a 1 min isothermal hold with a hydrogen carrier gas velocity of 50 cm/s. The test mixture contained 10 n-decane, Cg-NH = l-aminooctane, PY 3,5-dimethylpyrimidine, C 2 n-dodecane, - 1-amlnodecane, DMA ...

One of the major practical problems to the installation of HPLC as a permanent process monitor is the need to replace solvent. A large solvent reservoir may present problems both in terms of size and safety. One solution is the use of packed capillary columns, which consume much less solvent than conventional columns, as the comparison (at constant linear velocity) in Table 1 shows. 

Correlation was found between domain size and attainable column efficiency. Column efficiency increases with the decrease in domain size, just like the efficiency of a particle-packed column is determined by particle size. Chromolith columns having ca. 2 pm through-pores and ca. 1pm skeletons show H= 10 (N= 10,000 for 10 cm column) at around optimum linear velocity of 1 mm/s, whereas a 15-cm column packed with 5 pm particles commonly shows 10,GOO-15,000 theoretical plates (7 = 10—15) (Ikegami et al., 2004). The pressure drop of a Chromolith column is typically half of the column packed with 5 pm particles. The performance of a Chromolith column was described to be similar to 7-15 pm particles in terms of pressure drop and to 3.5 1 pm particles in terms of column efficiency (Leinweber and Tallarek, 2003 Miyabe et al., 2003). Figure 7.4 shows the pressure drop and column efficiency of monolithic silica columns. A short column produces 500 (1cm column) to 2500 plates (5 cm) at high linear velocity of 10 mm/s. Small columns, especially capillary type, are sensitive to extra-column band... 

Molecular diffusion (the B term) applies to both packed and capillary columns and derives from the fact that all molecules in the gas phase will diffuse into any available space. It is minimized by using an increased flow rate (see the carrier gas velocity in the denominator) and by using a high molecular weight carrier gas. 

In order to perform qualitative and quantitative analysis of the column effluent, a detector is required. Since the column effluent is often very low mass (ng) and is moving at high velocity (50-100 cm/s for capillary columns), the detector must be highly sensitive and have a fast response time. In the development of GC, these requirements meant that detectors were custom-built they are not generally used in other analytical instruments, except for spectroscopic detectors such as mass and infrared spectrometry. The most common detectors are flame ionization, which is sensitive to carbon-containing compounds and thermal conductivity which is universal. Among spectroscopic detectors, mass spectrometry is by far the most common. 

Methane is commonly used as a marker for measuring the gas holdup time (tm), which was done on a capillary column 25 m long by 0.25 mm ID by 0.25 pm film thickness. A retention time for methane of 1.76 min was obtained. Determine the average linear gas velocity (v) and the average volumetric flow rate (Fc). Explain how these values differ from the actual velocity and flows at the column inlet and outlet. 

The main bottleneck in the further development of CEC is related with the state of the art of the column manufacturing processes and the robustness of the columns/instrumentation. Moreover, evidence to demonstrate reproducibility of separations from column to column still has to be established. The formation of bubbles in the capillaries due to the Joule heating and variations in EOF velocity on passing from the stationary phase through the frit and into the open tube is still very challenging in packed column CEC. A way to overcome this problem is to use monolithic columns or apply open tubular CEC [108]. Currently, many efforts are placed in improving column technology and in the development of chip-CEC [115] as an attractive option for lab-on-a-chip separations. 

Column lengths, elution times, and back pressures are given for a capillary column affording 50,000 plates at a mobile phase velocity of 2 mm/s. b The back pressure exceeds capabilities of commercial instrumentation (typically 40 MPa). 

Fig. 26. Effect buffer concentration in the mobile phase on EOF velocity (1) and current (2). (Reprinted with permission from [ 110]. Copyright 2000 Elsevier). Conditions monolithic capillary column 75 pm i.d., total length 30 cm, active length 25 cm, containing sol-gel bonded 3 pm ODS/SCX with 80 A pores, mobile phase 70 30 acetonitrile/phosphate buffer pH 3.0, electric field strength 442 V/cm (voltage 15 kV)...

Fig. 28. Effect of pH of the mobile phase on linear flow velocity (1) and electrical current (2) in the monolithic capillary column. (Reprinted with permission from [149]. Copyright 1998 American Chemical Society). Conditions monolithic capillary column 100 pm i. d. 30 cm, mobile phase 80 20 acetonitrile/5 mmol/1 phosphate buffer, pH adjusted by addition of concentrated NaOH, flow marker thiourea 2 mg/ml, UV detection at 215 nm, voltage 25 kV, pressure in vials 0.2 MPa, injection, 5 kV for 3 s...

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