Evaluation of a PTV injector for quantitative analysis of volatile compounds at low concentrations

The performance of a PTV injector operated in the solvent venting mode with Tenax in the glass insert was evaluated with synthetic mixtures containing 5 to 50 ng of n-alkanes, ethyl esters, n-alcohols, and carboxylic acids. The influence of the sampled amount, the injected volume, and the nature of the solvent on accuracy and precision were studied. Coefficients of variation of relative (normalized) peak areas and absolute peak area ratios of each compound to the standard are of the order of 5 %.     

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.     

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.     

Determination of polycyclic aromatic hydrocarbons (PAHs) in particulate matter collected with low volume samplers

The determination of polycyclic aromatic hydrocarbons (PAHs) contained in samples of particulate matter (PM), collected with low volume pumps, were carried out with an high sensitivity method that comes from several revisions of a previous method. The present work describes how, by using programmable temperature vaporization (PTV) and a mass selective detector with inert ionic source for the GC-MS analysis and the modifications of microwave-assisted extraction (MAE), the sensitivity of the method can be increased.The PAHs chosen for testing the method are: benzo[a]anthracene (BaA), benzo[b]fluoranthene (BbF), benzo[k]fluoranthene (BkF), benzo[a]pyrene (BaP), indeno[1,2,3-cd]pyrene (Ip) and dibenzo[a,h]anthracene (DbA). They, in fact, belong to that group of substances that are the most harmful for human health for their carcinogenicity.PAHs recoveries for spiked standard solutions at different concentrations were between 95 and 100% with relative standard deviation ranging from 1 to 3%. The revised method was validated using a 1649a urban dust standard reference material (SRM). The results obtained were in good agreement with certified values. The high sensitivity of the method allows to carry out analyses using only a half of the sampled filter (usually 47 mm diameter membranes). In this way, the other half can be used for the characterization of the other components of PM (heavy metals, organic carbon, ions, etc). The last step has been constituted by application of the optimized method on real samples collected in two cities located in Southern Italy (Bari and Taranto).     

Programmed Temperature Vaporization Injection (PTV) in the Analysis by Gas Chromatography-Mass Spectrometry (GC-MS) of the Constituents of Landfill Gas

Abstract

Trace volatile compounds emitted from both domestic and industrial landfills have been identified by programmed temperature vaporization injection (PTV) coupled to gas chromatography with detection by ion-trap mass spectrometry (GC-ITD/MS). The PTV injection system has been developed using a combination of two six-port valves to achieve problems of interference in GC-MS while loading sample. A large volume of landfill gas was re-concentrated onto a sorbent trap, then rapidly liberated into the GC-ITD/MS system by programmed thermal desorption. Using this method, trace volatile compounds in gases from both domestic and industrial landfills such as aromatic hydrocarbons, terpenes, chlorinated hydrocarbons, and sulfur compounds can be identified and quantified.     

Book reviews

This work is a thorough investigation on the major operating parameters of the programmable temperature vaporisation (PTV) inlet used for gas chromatographic injection, including injection mode and volume, inlet temperature, vent and purge flow rates. The results clearly demonstrate the advantage of large volume injection in enhancing the detection of polybrominated diphenyl ethers (PBDEs). Partial loss of injected PBDEs occurred during solvent venting and due to incomplete sample transfer. Such loss was minimised by lowering the initial inlet temperature and vent flow and elevating the final inlet temperature. The results show that 50 mL/min vent flow, as low as 0°C initial and higher than 300°C final inlet temperatures produced the relatively high responses. Two mass spectrometric parameters were also evaluated. Indoor dust, lake sediment and human placenta tissue samples were analysed to demonstrate reliability and sensitivity improvement of the PTV large volume injection.     

Development of GC–MS/MS method with programmable temperature vaporization large volume injection for monitoring of 17β-estradiol and 2-methoxyestradiol in plasma

Monitoring of estradiol and its metabolites in biological samples is essential for the accurate diagnosis of a number of endocrine diseases. In this study, a sensitive, precise and specific GC–MS/MS method for the quantification of 17β-estradiol (17-BE) and its main metabolite, 2-methoxyestradiol (2-MEOE), in plasma was developed and validated. Plasma concentrations of these steroids are currently investigated as diagnostic markers for pre-eclampsia, a systematic disorder of pregnancy and a leading cause of maternal and fetal morbidity and mortality worldwide.     

Effects of fine fuel droplets on a laminar flame stabilized in a partially prevaporized spray stream

A partially prevaporized spray burner was developed to investigate the interaction between fuel droplets and a flame. Monodispersed partially prevaporized ethanol sprays with narrow diameter distribution were generated by the condensation method using rapid pressure reduction of a saturated ethanol vapor–air mixture. A tilted flat flame was stabilized at the nozzle exit using a hot wire. Particle tracking velocimetry (PTV) was applied to measurements of the droplet velocity; the laminar burning velocity was obtained from gas velocity derived from the droplet velocity. Observations were made of flames in partially prevaporized spray streams with mean droplet diameters of 7 μm and the liquid equivalence ratios of 0.2; the total equivalence ratio was varied. In all cases, a sharp vaporization plane was observed in front of the blue flame. Flame oscillation was observed on the fuel-rich side. At strain rates under 50 s⁻¹, the change in the burning velocity with the strain rate is small in fuel-lean spray streams. In spray streams of 0.7 and 0.8 in the total equivalence ratio, burning velocity increases with strain rates of greater than 50 s⁻¹. However, in spray streams with 0.9 and 1.0 in the total equivalence ratio, burning velocity decreases as the strain rate increases. At strain rates greater than 80 s⁻¹, burning velocity decreases with an increased gas equivalence ratio. The effect of mean droplet diameter, and the entry length of droplets into a flame on the laminar burning velocity, were also investigated to interpret the effect of the strain rate on the laminar burning velocity of partially prevaporized sprays.     

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.