Temperature-Programmed Injection

Obtain chromatograms of the three standards and also the pure gasoline (0% added). Give the column plenty of time to clear between injections—temperature programming may be useful. 

CP 9002, 50 m length, 0.32 mm ID CP-SIL 5 CB column with pre-column 1 m, 0.32 mm ID, carrier gas He split injection temperature program 45-300 °C, 4°C/min FID detector. Heptane correlation ratios (ratios Cj to C5) were calculated according to the method developed by Halpern (1995). 

Figure 12.7 Cliromatograms of a polycarbonate sample (a) microcolumn SEC ti ace (b) capillary GC ti ace of inti oduced fractions. SEC conditions fused-silica (30 cm X 250 mm i.d.) packed with PL-GEL (50 A pore size, 5 mm particle diameter) eluent, THE at aElow rate of 2.0ml/min injection size, 200 NL UV detection at 254 nm x represents the polymer additive fraction ti ansfeired to EC system (ca. 6 p-L). GC conditions DB-1 column (15m X 0.25 mm i.d., 0.25 pm film thickness) deactivated fused-silica uncoated inlet (5 m X 0.32 mm i.d.) temperature program, 100 °C for 8 min, rising to 350 °C at a rate of 12°C/min flame ionization detection. Peak identification is as follows 1, 2,4-rert-butylphenol 2, nonylphenol isomers 3, di(4-tert-butylphenyl) carbonate 4, Tinuvin 329 5, solvent impurity 6, Ii gaphos 168 (oxidized). Reprinted with permission from Ref. (14).

There are several types of sample introduction systems available for GC analysis. These include gas sampling valves, split and splitless injectors, on-column injection systems, programmed-temperature injectors, and concentrating devices. The sample introduction device used depends on the application. 

Programmed Temperature Injectors The programmed temperature injector is held near the boiling point of the solvent after injection of the sample, it is temperature programmed rapidly until it reaches the desired maximum temperature, which is normally higher than that of an isothermal (constant temperature) injector. As the sample components vaporize, they are transferred onto the head of the GC column. This technique is a varia-... 

The use of a fused silica capillary column for the GC analysis of the neutral oil extract has provided the means for improving the resolution of components in a more inert system. The sultones are determined by temperature-programmed GC over CP-Sil-5 CB (methyl silicone fluid) in a 25 m x 0.2 mm fused silica capillary column using nonadecane as internal standard. A sample split ratio of 1 100 is recommended for a 3-pl injection. 

Immediately after injection, heat the oven to 40 C (for very thin films to 30 C) and start the temperature program. 

Cool on-column Liquid sample is directly and totally passed from syringe into column or its extension. Cold injection followed by temperature program Dilute, thermally labile samples high-boiling components Fair, some focusing required 0.1-1 100... 

Although cSFC shows relatively poor figures of merit (speed, sensitivity, detection dynamic range and sample capacity) as well as a limited application area, its applications tend to be unique. These include solutes that can be solvated with pure SCCO2 and quantified with FID. Linear density programs typical in cSFC are ideal for homologous series found in surfactants, many prepolymers, etc. Selectivity in cSFC, which can be achieved by mobile phase density and temperature programming, relies on selective interactions with the stationary phase. Quantitative analysis in cSFC may be rendered difficult by small injected volumes the use of internal standards is recommended. 

The second part of this work will be dedicated to the start of the game what are the pieces motions How can the adsorbed molecules react on the surface and among all the playground, where does the real action take place This is the so-called in situ approach for which techniques such as temperature-programmed surface reaction (TPSR) or transient analysis by pulse injection have been developed. 

Figure 5.19 Formation of amino acids on ice surfaces irradiated in the laboratory (Nature Nature 416, 403-406 (28 March 2002) doi 10.1038/416403a-permission granted). Data were obtained from analysis of the room temperature residue of photoprocessed interstellar medium ice analogue taken after 6 M HCl hydrolysis and derivatization (ECEE derivatives, Varian-Chrompack Chirasil-L-Val capillary column 12 m x 0.25 mm inner diameter, layer thickness 0.12 pirn splitless injection, 1.5 ml min-1 constant flow of He carrier gas oven temperature programmed for 3 min at 70°C, 5°C min-1, and 17.5 min at 180°C detection of total ion current with GC-MSD system Agilent 6890/5973). The inset shows the determination of alanine enantiomers in the above sample (Chirasil-L-Val 25 m, single ion monitoring for Ala-ECEE base peak at 116 a.m.u.). DAP, diaminopentanoic acid DAH, diaminohexanoic acid a.m.u., atomic mass units.

Unexpected peaks can arise from components from a previous injection that moved slowly through the column, contamination from either the reagents used to prepare the sample or the standards, or a contaminated septum, carrier, or column. Solutions to these problems include a rapid bakeout via temperature programming after the analyte peaks have eluted, use of pure reagents, and replacement or cleaning of septa, carrier, or column. 

The analyte solution is placed (injected) into the furnace with a micropipet or auto-sampler. Following this, a temperature program is initiated in which the furnace heats rapidly to 1) evaporate the solvent, 2) char the solid residue, and finally 3) atomize the analyte, creating the atomic vapor. 

Automatic operation of the metering pump allows repetitive injections with unattended operation. Precise control of the carrier-gas flow ensures stable chromatograms and reproducible timings for collection of samples. Independent column oven and vaporizer temperatures are available up to 300°C and these can be operated with temperature programming or isothermally. The latter option is the most common. 

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