Supercritical fluid extraction-capillary gas chromatography: On-line coupling with a programmed temperature vaporizer

A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative transfer of solutes to the seperation column. The problems caused by impurities in the extraction fluid in on-line SFE-GC are discussed. Simple methods are described for the purification of commercially available carbon dioxide. The trapping efficiency of the PTV injector is studied. Applications of the SFE-PTV-GC system are given for the analysis of polymer anti-degradants, polar compounds, and samples with environmental relevance.     

Investigation of parameters affecting the on-line combination of supercritical fluid extraction with capillary gas chromatography

Two different injectors, a split/splitless injector and a programmed temperature vaporizer (PTV) injector were investigated as the interface in on-line supercritical fluid extraction (SFE)-capillary gas chromatography (cGC). The parameters affecting the chromatographic peak shapes as well as the quantitative performance of the interfaces in on-line SFE-cGC were identified and studied. Particular attention was paid to the case where modified extraction fluids were used. Experiments were performed on two different samples. The first sample consisted of PAHs spiked on sand at different concentration levels. The other sample was a polymeric material.     

Improved method for the determination of sulfur components in natural gas

Determination of trace concentrations of sulfur components in natural gas is a true analytical challenge. Only analytical procedures based on gas chromatography can meet the sensitivity and accuracy requirements dictated by environmental regulation institutions and modern chemical industry. In the present contribution the sample pretreatment and chromatographic separation steps have been evaluated and optimized based on the use of a flamebased sulfur chemiluminescence detector (SCD) for target compound detection. The proposed instrument consists of a programmed temperature vaporizing (PTV) injector employing a liner packed with Chromosorb 104, a 4 μm thick film apolar column and a flame-based SCD. Using a 13 mL sample loop the detection limit achievable with the new method is 3 μg S/m³. The precision of replicate measure. ments is generally in the range of 5–15% relative standard deviation. Lower detection limits can be achieved by preconcentrating larger sample volumes, e.g. 100 mL.     

Large-volume PTV injection: Comparison of direct water injection and in-vial extraction for GC analysis of triazines

Summary The potential of large-volume PTV injection was studied for the analysis of triazine herbicides in water samples. Direct water injection and in-vial extraction were described and compared. Detection limits were between 0.01–0.02 μg L⁻¹ and relative standard deviations were <9%. Both methods are suitable for the analysis of triazines at ppt-level, although in-vial extraction is favourable for water samples with relatively large amounts of matrix components.     

Analysis of triglycerides by capillary gas chromatography with programmed-temperature injection

The capillary gas chromatographic analysis of complex naturally occurring and food-product triglyceride mixtures is accomplished qualitatively and quantitatively on columns coated with methyl and methyl-phenyl (65%) silicones using programmed-temperature split/splitless and on-column injection. Faster analysis times are achieved using elevated initial column oven temperatures with cold initial injector temperatures.     

Comparison of different injection modes in edible oil minor components analysis

Waxes and fatty acid alkyl esters are minor components used as official parameters to control the authenticity and quality of a high‐value olive oil product. A poor measurement can lead to a misleading classification of the oil. The official method requires their analysis together by capillary gas chromatography equipped with a flame ionization detector and an on‐column injector to avoid discrimination and thermal degradation. The degradation can occur to a different extent if different (and not properly optimized) injectors are used. However, other injection techniques, such as programmed‐temperature vaporizer, are much more versatile and more widespread. The aim of the present work was to compare the performance of a programmed‐temperature vaporizer injector, in on‐column and splitless mode, with the on‐column injector to analyze alkyl esters and waxes. Discrimination among high‐boiling compounds was evaluated, as well as the occurrence of thermal degradation, especially of sterols and diterpene alcohol (phytyl and geranylgeraniol) esters. A proper optimization of a programmed‐temperature vaporizer injection, with particular attention to the liner selection, was proven to provide comparable results to the traditional on‐column injection. A performance comparison was carried out both on standard mixtures and on real oil samples.     

Rapid simultaneous determination of multiple pesticide residues in traditional Chinese medicines using programmed temperature vaporizer injection-fast gas chromatography coupled with mass spectrometry

A fast gas chromatography coupled with mass spectrometry (GC-MS) using large volume injection with programmed temperature vaporizer in solvent vent mode (PTV-LVI-SV) was developed for the trace determination of multiple pesticide residues in traditional Chinese medicines (TCMs). Experimental conditions of PTV-LVI-SV injection were optimized by central composite design. The optimized result was that initial temperature was held at 40°C for 39 s, vent flow rate was set at 45 mL/min and vent pressure was held at 0 psi for 36 s, injection volume was 10 μL. Furthermore, the quick and effective QuEChERS (quick, easy, cheap, effective, rugged and safe) method was performed to extract and purify pesticide residues in TCMs. The prepared samples were analyzed with GC-MS in the selected ion monitoring mode (SIM). The lowest LOD was 4 μg/kg for some pesticides. The recoveries were checked by spiking samples with pesticides at 25, 50 and 250 μg/kg. The average recoveries of most pesticides were from 80 to 118%. The result indicated that QuEChERS and PTV-LVI-SV GC-MS method was a rapid and sensitive analysis technique for the determination of multiple pesticide residues in TCMs.     

空温式翅片管气化器非稳态结霜速率分析

观测了某实际运营的空温式翅片管气化器附近湿空气流动状态。基于热力学理论和湿空气流动状态建立了空温式翅片管气化器表面非稳态结霜模型,推导了非稳态结霜速率的关系式,分析了不同工况下非稳态结霜速率影响因素。非稳态结霜速率随湿空气温度、相对湿度和气流速度增加而增加,其主要影响因素为湿空气温度和相对湿度,而气流速度影响相对较小。非稳态结霜速率分析为精确计算空温式翅片管气化器传热特性提供了一定理论依据。     

A universal sample injection system for capillary column GC using a programmed temperature vaporizer (PTV)

This article describes the use of a programmed temperature vaporizer injection system which overcomes many of the classical problems associated with other injection techniques employed in capillary GC. The system can be operated in three distinct modes.     

AT-column, a novel concentrating technique for large-volume injections in gas chromatography

Nowadays, large-volume injection is widely used for the GC determination of trace analytes, specifically to improve detectability. The most popular injectors for large-volume injections are the programmable temperature vaporisation (PTV) injector and the cold on-column (COC) injector, where each device has its own advantages and limitations. The novel AT-column concentrating technique combines features of two other injection techniques, loop-type large-volume and vapour overflow. AT-column injection is based on solvent evaporation in an empty liner with solvent vapour discharge via the split line. Little or no optimisation is required. The only relevant parameter is the injection temperature which can easily be calculated using the equation of Antoine. As an application, AT-column injection is combined with GC-MS for the trace-level determination of labile analytes and with GC-flame ionisation detection for the analysis of high molecular weight polymer additives. In summary, AT-column is an injection technique that combines the inertness of the COC, and the flexibility and robustness of the PTV large-volume technique.