Combination with capillary gas

Shen Y, Jdnsson jA, and Mathiasson L. On-line microporous membrane liquid-liquid extraction for sample pretreatment combined with capillary gas chromatography applied to local anesthetics in blood plasma. Anal. Chem. 1998 70 946-953. 

A desirability function was established to optimise the working conditions of a headspace solid-phase microextraction step, combined with capillary gas chromatography and ICP. 

Analysis for the butanals is most conveniendy carried out by gas chromatography. Trace quantities of -butyraldehyde (18 ppb) in exhaust gases have been determined employing a combination of capillary gas chromatography with thermionic detection (35). Sinulady, trace amounts of -butyraldehyde in cigarette smoke and coffee aroma have been determined by various capillary gc techniques (36,37). 

Figure 2.19 Schematic representation of an on-line liquid-liquid extraction-GC/AED system. Reprinted from Journal of High Resolution Chromatography, 18, E. C. Goosens et al, Continuous liquid-liquid extraction combined on-line with capillary gas chromatography- atomic emission detection for environmental analysis , pp. 38-44, 1995, with permission from Wiley-VCH.

X. Lou, H.-G. Janssen and C. A. Cramers, Investigation of parameters affecting the online combination of supercritical fluid extraction with capillary gas chromatography , J. Chromatogr. 750 215-226 (1996). 

Catalytic tests in sc CO2 were run continuously in an oil heated flow reactor (200°C, 20 MPa) with supported precious metal fixed bed catalysts on activated carbon and polysiloxane (DELOXAN ). We also investigated immobilized metal complex fixed bed catalysts supported on DELOXAN . DELOXAN is used because of its unique chemical and physical properties (e. g. high pore volume and specific surface area in combination with a meso- and macro-pore-size distribution, which is especially attractive for catalytic reactions). The effects of reaction conditions (temperature, pressure, H2 flow, CO2 flow, LHSV) and catalyst design on reaction rates and selectivites were determined. Comparative studies were performed either continuously with precious metal fixed bed catalysts in a trickle bed reactor, or discontinuously in stirred tank reactors with powdered nickel on kieselguhr or precious metal on activated carbon catalysts. Reaction products were analyzed off-line with capillary gas chromatography. 

The successful application of the CFD method in combination with subsequent gas chromatographic separation and the use of an BCD has resulted in the extensive development of this technique. However, other CFD methods aimed at obtaining derivatives that can be selectively detected by other selective detectors (e.g., sodium thermionic, flame photometric) have not been developed adequately, despite their obvious promise. It seems that the high selectivity of the method should be used for the elaboration of selective methods of functional group analysis in order to identify compounds at the picogram level. This is especially pertinent to the analysis of microsamples on capillary columns. 

Steroids from Plasma and Identification with the Combination Glass Capillary Gas Chromatography-Mass Spectrometry... 

Jackson and Walker studied the applicability of pyrolysis combined with capillary column gas chromatography mass spectrometry to the examination of phenyl polymers (eg. styrene-isoprene copolymer) and polymer like phenyl ethers (eg. bis(m-(m-phenoxy phenoxy)phenyl)ether). They examined the effect of varying parameters affecting the nature of products formed and relative product distribution in routine pyrolysis. These parameters include the effects of pyrolysis temperature rise times, pyrolysis temperatures up to 985 C and pyrolysis duration. Temperature rise time (0.1 to 1.5 s) is not a critical factor in the Curie point pyrolysis of a styrene-isoprene copolymer, either with regard to the nature of the products formed or their relative distributions. Additionally, the variation of pyrolysis duration or hold time (2.0 to 12.5 s) at a fixed Curie temperature reflected no change in the nature of components formed however changes in product distributions were observed. Variations in Curie temperature at a fixed pyrolysis duration produced drastic changes in product distributions such as a three-... 

The advent of high-resolution capillary gas chromatography (HR-CGC) with on-column injection has resulted in improved GC analysis of polymer additives [92-94]. The solution of the additive mixture is injected directly into the cold end of the capillary column by means of a cold injector. Thus, sample discrimination, the instantaneous evaporation of the sample solvent, is avoided. The nonvaporising, on-column injection combined with very high resolution of the capillary columns allows accurate separation, identification and quantification of additives of complex mixtures. With the solvent venting technique, the sample is introduced into the column without splitting and sample concentrations... 

That boiling produces bubbles of vapor creates an additional problem for performing the experiment. If a bubble of gas forms at the bottom of a capillary tube, its expansion and rise to the top of the capillary will expel the rest of the liquid. This is due to the fact that the surface tension of most liquids combined with the narrow bore of the capillary will not allow fluid to drain around the bubble as it rises. The solution is that a larger sample tube and sample is required for the experiment. One advantage of the boiling point experiment is that the thermal conductivity of a liquid is higher than its solid because of the mobility of the molecules. 

Mass transfer (the C term), which involves collisions and interactions between molecules, applies differently to both packed and capillary columns. Packed columns are mostly filled with stationary phase so liquid phase diffusion dominates. The mass transfer is minimized by using a small mass of low-viscosity liquid phase. Capillary columns are mostly filled with mobile phase, so mass transfer is important in both the gas and liquid phases. A small mass of low-viscosity liquid phase combined with a low-molecular weight carrier gas will minimize this term. 

The most commonly used methods for measuring mirex in blood, tissues (including adipose tissue), milk, and feces are gas chromatography (GC) or capillary GC combined with electron capture detection (ECD) or mass spectrometry (MS). Tables 6-1 and 6-2 summarize the applicable analytical methods for determining mirex and chlordecone, respectively, in biological fluids and tissues. 

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