Capillary column selection factors

Chemical Analysis of Extracts. The extracts were analyzed by capillary column GC-MS for OCs, TAAPs, and PAHs (see the list on page 313). The GC-MS parameters used at the two laboratories are shown in Table II. The identification and quantitation were all done by using automatic routines based on a mass spectra library created from authentic standards of the selected compounds. Compounds were located by searching the reconstructed ion chromatogram for each library entry within a narrow retention time window relative to the internal standard (anthracene-dio or phenanthrene-dio). Quantitation was achieved by comparison of characteristic ion areas in the field samples with ion areas of the internal standard. These ion areas were normalized by response factors established by comparison of ion ratios of a standard mixture of all 66 analytes at a concentration of 2.5 ng//zL. 

Tests of the reproducibility of retention times, retention factors, separation selec-tivities, and column efficiencies for our methacrylate monolithic capillary columns are summarized in Table 6.2. This table shows averaged data obtained for 9 different analytes injected 14 times repeatedly every other day over a period of 6 days, as well as for 7 different capillary columns prepared from the same polymerization mixture. As expected, both injection-to-injection and day-to-day reproducibilities measured for the same column are very good. Slightly larger RSD values were observed for col-umn-to-column reproducibility. While the selectivity effectively did not change, larger differences were found for the efficiencies of the columns. 

The NMR spectra were recorded on Bruker AC200 (200 MHz) and AC300 (300 MHz) spectrometers at ambient temperature in NMR solvents obtained from ISOTEC Inc.. G.C. analysis were performed on Unicam PU4600 and PU610 apparatus with 30 m J W Scientific DB-1, DB-17 and AT-SILAR capillary columns and flame ionization detectors. Product yields were determined by peak area analysis response factors for selected substrates and products were foimd to be virtually identical. Internal standards were used in the initial stage of this study, but were found to influence the catalyst characteristics. G.C.M.S. was performed on a Unicam Automass apparatus combined with 610 series G.C. apparatus equipped with 30 m J W Scientific DB-1 and DB-17 columns. TEM-EDAX was performed on a Phillips CM 200 microscope equipped with a field emission gun. TEM-EDAX samples were prepared by application of a few droplets of a suspension of the catalyst in ethanol onto a holey carbon film which was supported by a nickel grid after which the ethanol was allowed to evaporate. 

The GC-FID analysis is conducted by injection of 1 to 2 fil of FI or F3 into a gas chromatograph equipped with a high resolution capillary column (operated in sphtless injection mode). The injector and detector temperatures are set at 290 and 300°C, respectively. The GC temperature program is selected to achieve near-baseline separation of all of the saturated hydrocarbons. Quantitation of the individual components is performed by the internal standard method. The relative response factor (RRF) for each component is calculated relative to the internal standard. The TPH is also quantified by the internal standard method using the baseline corrected total area of the chromatogram and the average hydrocarbon response factor determined over the entire analytical range. ... 

Liquid samples were regularly withdrawn with a filtering syringe and analyzed by a gas chromatograph (Perkin Ehner) equipped with an FID detector and using a capillary column (CPSilSCB, 25 m). All the isomers (Z, E) of crosscondensation and self condensation reactions have been separated and identified by H-NMR and GC-MS. Quantitative determinations were based on the measured response factors of the reactants and reaction products. We checked that reactions were carried without transfer limitations. The selectivity for a particular product was defined as the mmol of this product divided by the total mmol of heptanal converted. 

GC/MS with capillary columns has been the gold standard for more than 20 years, but LC/MS has become a complementary method due to the success in interface development with atmospheric pressure ionisation (API) for low molecular weight compounds and the appHcation to biopolymers. For many areas of analytical chemistry, LC/MS has become indispensible due to its advantages over GC/MS for polar and thermolabile analytes. A Hmiting factor for LC/MS has been the incompatibility between the hquid eluting from the LC and the mass spectrometer vacuum. This could be overcome in electrospray ionisation with the use of a nebuliser gas ( ion spray ) or additional heated drying gas ( turbo ion spray ) (70, 71]. Due to its high sensitivity and selectivity, APl-MS has become a standard tool for the stracture elucidation of analytes from complex mixtures. 

Factors Controlling Selectivity Open Tubular Columns Dynamic Coating Static Coating Column Regeneration Capillary Column Design and Choice Stationary Phases for the GC Separation of Chiral Substances Synopsis References Chapter 6... 

Anything that increases the column efficiency N, the column selectivity a. or the retention factor k will enhance the separation power of the column. Packed columns are characterized by low plate numbers and PCGC is therefore a low-resolution technique. The lower efficiency is compensated by the high. selectivity a of the stationary phase, and this is the main reason why so many different stationary pha.ses have been developed for PCGC. Capillary columns on the other hand have very high plate numbers and, therefore, the number of stationary phases can be restricted because the selectivity is less important. In fact, most separation problems can be handled with four basic. stationary pha.ses and half a dozen tailor-made stationary phases. Other important features of capillary columns are their inertness and compatibility with spectroscopic detectors. In the framework of this discussion, emphasis is, therefore, on capillary columns. 

---