Chromatographic determination transfer

Eire protection - Eire extinguishing media - Elalogenated hydrocarbons. Code of practice for safe handling and transfer procedures. Supersedes BS 6535 Section 2.2 1989 Water quality - Gas chromatographic determination of some selected chlorophenols m water. Also BS 6068-2.65 1999... 

Pass the solution derived from Section 6.2.2 through a Cig cartridge (conditioned prior to use successively with 5mL of acetonitrile and 10 mL of water), then elute interfering substances with 15 mL of acetonitrile-water (3 17, v/v) and discard the eluate. Elute imibenconazole-debenzyl with 20 mL of acetonitrile-water (2 3, v/v) and collect the eluate in a 100-mL separatory funnel (imibenconazole-debenzyl fraction). Elute imibenconazole with 20 mL of acetonitrile-water (17 3, v/v) and collect the eluate in a 100-mL separatory funnel (imibenconazole fraction). Add 30 mL of 20% sodium chloride aqueous solution and 40 mL of ethyl acetate to each separatory funnel and shake the funnel with a mechanical shaker for 5 min. Collect the ethyl acetate extract, dry the extract with anhydrous sodium sulfate and transfer into a 100-mL round-bottom flask. Concentrate the ethyl acetate extract to near dryness by rotary evaporation and dry with a stream of nitrogen. Dissolve the residue of each fraction in acetone for gas chromatographic determination as in Section 6.3. 

This azole transfer has been used for expedient gas chromatographic determination of 2-ethylhexanoic acid.[34]... 

Chen S-H, Wu S-M, Kou H-S, et al. 1994. Electron-capture gas chromatographic determination of cyanide, iodide, nitrite, sulfide and thiocyanate anions by phase-transfer-catalyzed derivatization with pentafluorobenzyl bromide. J Anal Toxicol 18(2) 81-85. 

Dolan and Hall [148] have described a Coulson electrolytic conductivity detector of enhanced sensitivity for the gas chromatographic determination of chlorinated insecticides in the presence of PCBs. The detector was modified by the replacement of the silicone-rubber septum and stainless steel fitting at the exit of the pyrolysis furnace with PTFE fitting, by the reduction in diameter of the PTFE transfer tube, and by the... 

Lmdqvist L and Maenpaa, P. H (1982) Gas chromatographic determination of ammo acids and ammo acids attached to transfer RNA m biological samples. J Chromatogr. 232, 225-235. 

To determine how the height of a theoretical plate can be decreased, it is necessary to understand the experimental factors contributing to the broadening of a solute s chromatographic band. Several theoretical treatments of band broadening have been proposed. We will consider one approach in which the height of a theoretical plate is determined by four contributions multiple paths, longitudinal diffusion, mass transfer in the stationary phase, and mass transfer in the mobile phase. 

In the analytical chromatographic process, mixtures are separated either as individual components or as classes of similar materials. The mixture to be separated is first placed in solution, then transferred to the mobile phase to move through the chromatographic system. In some cases, irreversible interaction with the column leaves material permanently attached to the stationary phase. This process has two effects because the material is permanently attached to the stationary phase, it is never detected as leaving the column and the analysis of the mixture is incomplete additionally, the adsorption of material on the stationary phase alters the abiHty of that phase to be used in future experiments. Thus it is extremely important to determine the ultimate fate of known materials when used in a chromatographic system and to develop a feeling for the kinds of materials in an unknown mixture before use of a chromatograph. 

Table 8-10 gives pertinent data for the Menschutkin reaction of triethylamine with ethyl iodide. These reactant molecules are volatile, so their transfer free energies were determined by a gas chromatographic variation of the vapor pressure method. For this reaction Eq. (8-57) is written... 

Mondello et al. (2, 20-23) have used a multidimensional gas chromatographic system based on the use of mechanical valves which were stable at high temperatures developed in their laboratory for the determination of the enantiomeric distribution of monoterpene hydrocarbons (/3-pinene, sabinene and limonene) and monoterpene alcohols (linalol, terpinen-4-ol and a-terpineol) of citrus oils (lemon, mandarin, lime and bergamot). Linalyl acetate was also studied in bergamot oil. The system consisted of two Shimadzu Model 17 gas chromatographs, a six-port two-position valve and a hot transfer line. The system made it possible to carry out fully... 

The effects of various pore-size distributions, including Gaussian, rectangular distributions, and continuous power-law, coupled with an assumption of cylindrical pores and mass transfer resistance on chromatographic behavior, have been developed by Goto and McCoy [139]. This study utilized the method of moments to determine the effects of the various distributions on mean retention and band spreading in size exclusion chromatography. 

Figure 8.26(A) is an example of a valve type interface [329]. Helium carrier gas is provided to the headspace saiq)ler and is split into two flow paths. One path is flow-controlled and provides a constant flow of carrier gas which passes from the headspace unit through the heated transfer line to the gas chromatograph. The second flow path is pressure-regulated and, in the standby mode, the seunple loop and seuapling needle are flushed continuously by the helium flow. At a time determined by the operator, the sampling needle pierces the septum and helium pressurizes the headspace vial to any desired pressure. The headspace gas is then allowed to vent through the sample loop. Once filled, the sample loop is placed in series with the normal carrier gas flow and its contents are driv Bbhrough the heated...

Trace analysis is particularly attractive for SFE-HPLC since quantitative transfer of all analytes extracted to the chromatographic system becomes possible. At present, on-line SFE-HPLC appears to be feasible for qualitative analysis only quantitation is difficult due to possible pump and detector precision problems. Sample size restrictions also appear to be another significant barrier to using on-line SFE-HPLC for quantitative analysis of real samples. On-line SFE-HPLC has therefore not proven to be a very popular hyphenated sample preparatory/separation technique. Although online SFE-HPLC has not been quantitatively feasible, SFE is quite useful for quantitative determination of those analytes that must be analysed by off-line HPLC, and should not be ruled out when considering sample preparatory techniques. In most cases, all of the disadvantages mentioned with the on-line technique (Table 7.15) are eliminated. On- and off-line SFE-HPLC were reviewed [24,128]. 

Another method to detect energy transfer directly is to measure the concentration or amount of acceptor that has undergone an excited state reaction by means other than detecting its fluorescence. For instance, by chemical analysis or chromatographic analysis of the product of a reaction involving excited A [117, 118]. An early application of this determined the photolyzed A molecules by absorption spectroscopic analysis. [119-121], This can be a powerful method, because it does not depend on expensive instrumentation however, it lacks real-time observation, and requires subsequent manipulation. For this reason, fluorescence is the usual method of detection of the sensitized excitation of the acceptor. If it is possible to excite the donor without exciting the acceptor, then the rate of photolysis of the acceptor (which is an excited state reaction) can be used to calculate the FRET efficiency [122],... 

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