Capillary sample introduction

A direct injection nebulizer has been used for CE-ICP-MS [101] with the capillary actually inserted through the central sample introduction capillary of the DEN (Fig. 10.17). This nebulizer is very well suited to the very low flow rates associated with CE and also offers approximately 100% sample transport efficiency. A platinum grounding electrode was used, situated in a three-port connector, which also accommodated the DEN capillary and a makeup buffer flow. The makeup buffer was used so that the DIN operation was independent of the EOF, and the two flows were combined at the capillary exit. The system was used for feasibility studies for As and Se speciation. 

H. G. Riepe, V. Loreti, R. Garcia-Sanchez, C. Camara, J. Bettmer, Removal of interfering elements in ICP-QMS for the determination of Pt, Rh, and Pd by chemically modi-bed sample introduction capillaries, Fresenius J. Anal. Chem., 370 (2001), 488 D491. 

OCN), which is a variation of the pneumatic concentric nebulizer built from flexible capillary mbes, was used in an interface. The OCN has had little application in CE interfaces, owing to its generally lower sensitivity performance when compared to other pneumatic nebulizers used with ICP-MS detection.The direct injection nebulizer (DIN), previously described in The Nebulizer, was used by Liu et al. in a CE interface. The electrophoretic capillary was directly inserted through the central sample introduction capillary of the DIN. A platinum grounding electrode was positioned into a three-port connector. This connector contained the DIN sample introduction capillary as well as a make-up buffer flow. These alternative nebulizers have been successfully used in CE interfaces, but the pneumatic designs dominate the interface systems reported in the literature. 

P. Sandra (Ed.), Sample Introduction in Capillary Gas Chromatography, Vol 1, Chromatographic Method Series, Huethig, Basel, 1985. 

Z. Fiu and J. B. Phillips, Sample introduction into a 5 p.m i.d. capillary gas chr omatog-raphy column using an on-column thermal desorption modulator , /. Microcolumn Sep. 1 159-162(1989). 

An exeuaple of a nodular apparatus for capillary electrophoretic separation methods, is shown in Figure 4.43 [637-639,681-684]. It Offers a choice of automated sample introduction methods with on-column detection and has a... 

P. Sandra, (Ed.), "Sample Introduction in Capillary Gas Chromatography", Huethig, Heidelberg, Vol. 1, 1985. 

Guttman, A. and Schwartz, H. E., Artifacts related to sample introduction in capillary gel electrophoresis affecting separation performance and quantitation, Anal. Chem., 34, 2279, 1995. 

Fang, Q., Wang, F.-R., Wang, S.-L., Liu, S.-S., Xu, S.-K., and Fang, Z.-L., Sequential injection sample introduction microfluidic-chip based capillary electrophoresis system, Anal. Chim. Acta, 390, 27, 1999. 

H.-G. Janssen, Sample Introduction Techniques for Capillary Gas Chromatography (Reference GI-12981), Gerstel Inc., Mulheim ad. Ruhr (1998). 

Principles and Characteristics As mentioned already (Section 3.5.2) solid-phase microextraction involves the use of a micro-fibre which is exposed to the analyte(s) for a prespecified time. GC-MS is an ideal detector after SPME extraction/injection for both qualitative and quantitative analysis. For SPME-GC analysis, the fibre is forced into the chromatography capillary injector, where the entire extraction is desorbed. A high linear flow-rate of the carrier gas along the fibre is essential to ensure complete desorption of the analytes. Because no solvent is injected, and the analytes are rapidly desorbed on to the column, minimum detection limits are improved and resolution is maintained. Online coupling of conventional fibre-based SPME coupled with GC is now becoming routine. Automated SPME takes the sample directly from bottle to gas chromatograph. Split/splitless, on-column and PTV injection are compatible with SPME. SPME can also be used very effectively for sample introduction to fast GC systems, provided that a dedicated injector is used for this purpose [69,70],... 

Fused silica capillary columns of various internal bores and of lengths in the range 25 to 50 m are mainly employed for analytical separations. A variety of polar and non-polar column types are available including those open tubular types with simple wall coatings (WCOT), those with coatings dispersed on porous solid-supports to increase adsorbent surface area (SCOT) and porous layer open tubular (PLOT) columns. Important stationary phases include polyethylene glycol, dimethylpolysiloxane and different siloxane copolymers. Various sample introduction procedures are employed including ... 

In contrast to sample introduction via direct probe (Chap. 5.3.1), the components eluting from a GC capillary are quantitatively transferred into the ion source during a short time interval just sufficient to acquire about five mass spectra. Consequently, the partial pressure of the analyte is comparatively high during elution allowing sample amounts in the low nanogram range to be analyzed by capillary GC-MS. 

Figure 3.7 Determination of the enantiomeric purity of SB-214857 API using CD-modified CE. Distomer content measured at 0.06% by area. (Conditions plain fused silica capillary, 50 cm effective length, 57 cm total length, 75 pm i.d. buffer lithium phosphate [pH 3.0, 100 mM] containing 0.05% (w/v) hydroxyethy[cellulose and 1.5 mM dimethyl- 8-CD voltage 30 kV temperature 20°C detection UV at 200 nm sample preparation 0.2 mg/ml in water sample introduction 5 s at 35 mbar, capillary inlet at anode.)...

Chen, G. and J. Wang. Fast and simple sample introduction for capillary electrophoresis microsystems. Analyst 129, 507-511 (2004). 

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