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Headspace Technique (headspace + technique)
Selected AbstractsREACH-driven developments in analysis and physicochemistry,FLAVOUR AND FRAGRANCE JOURNAL, Issue 3 2010A. Chaintreau Abstract The enforcement of the REACH regulation in the fragrance domain has created new challenges for the analytical and physical chemist. Many chemicals used as perfumery ingredients are hydrophobic, because low-polar compounds exhibit a higher substantivity (i.e. persistence after application) than do polar compounds. As a result, the usual protocols are often unsuitable and new methods must be developed. Biodegradation studies sometimes call for the quantification of traces of such hydrophobic analytes in complex media (e.g. waste water, aqueous surfactant solutions). Existing sample preparation techniques are either inefficient or time consuming. A new approach is proposed, based on single-use absorbants, which allows accurate quantification down to the 100 ppb range. This extremely simple technique allows good throughput analyses. Determining the environmental profile of a compound requires the determination of some physical constants. Among these, solubility in water can be obtained from theoretical models or experimentally, but the resulting values may greatly differ as a function of the model or the protocol. Several experimental approaches are critically discussed and compared with a reference technique. The air-to-water partition coefficients are determined by using an improved version of the previously developed static-and-trapped headspace technique. Copyright © 2009 John Wiley & Sons, Ltd. [source] Solid-phase aroma concentrate extraction (SPACEÔ ): a new headspace technique for more sensitive analysis of volatilesFLAVOUR AND FRAGRANCE JOURNAL, Issue 3 2004Masashi Ishikawa Abstract The SPACEÔ (solid-phase aroma concentrate extraction) method is a modi,ed version of the SPME (solid-phase micro extraction) technique for headspace analysis, with increased area of the adsorbent to enable more sensitive analysis of volatiles. The SPACEÔ rod used in the technique is fabricated from stainless steel coated with an adsorbent mixture, consisting mainly of a graphite carbon. Initially, the SPACEÔ rod is ,xed in the head of a closed ,ask, where it adsorbs the aroma. Next, the rod is thermally desorbed on-line with a high-resolution gas chromatography,mass spectrometer (HRGC,MS). In the present experiments, SPACEÔ sampling reproducibility was determined by analysing a standard mixture and roasted coffee beans. The SPACEÔ rod collected the analytes with good reproducibility, with the exception of high polar compounds. Similar analyses of coffee powder were performed by SPME and other methods for comparison with the SPACEÔ method. The SPACEÔ method proved to have superior capabilities with high concentrations, and it produced a well-balanced chromatogram. Copyright © 2004 John Wiley & Sons, Ltd. [source] Determination of polycyclic aromatic hydrocarbons in olive oil by a completely automated headspace technique coupled to gas chromatography-mass spectrometryJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 6 2006Francisco J. Arrebola Abstract A new and completely automated method for the determination of ten relevant polycyclic aromatic hydrocarbons (PAHs) in olive oil is proposed using an extraction by the headspace (HS) technique. Quantification and confirmation steps are carried out by gas chromatography-mass spectrometry (GC-MS) combining simultaneously selected-ion monitoring (SIM) and tandem mass spectrometry (MS/MS). This combination offers on one hand an increased sensitivity and on the other hand, selective and reliable qualitative information. Sample pretreatment or clean-up are not necessary because the olive oil sample is put directly into an HS vial, automatically processed by HS and introduced into the GC-MS instrument for analysis. Because of its high selectivity and sensitivity, a triple-quadrupole (QqQ) detector coupled with the gas chromatograph allows us to limit handling. Each sample is completely processed in approximately 63 min (45 min for HS isolation and 18 min for GC-MS determination), a reduced time compared with previously published methods. The chemical and instrumental variables were preliminarily optimized using uncontaminated olive oil samples spiked with 25 µg kg,1 of each target compound. The final method was validated to ensure the quality of the results. The precision was satisfactory, with relative standard deviation (RSD) values in the range 3,9%. Recovery rates ranged from 96 to 99%. Limits of detection (LOD) were calculated as 0.02,0.06 µg kg,1 and the limits of quantification (LOQ) were obtained as 0.07,0.26 µg kg,1. It must be mentioned that the LOD and LOQ are much lower than the maximum levels established by the European Union (EU) in oils and fats intended for direct human consumption or for use as an ingredient in foods, which are set at 2 µg kg,1. All the figures of merit are completely in accordance with the latest EU legislation. This fact makes it possible to consider the proposed method as a useful tool for the control of PAHs in olive oils. Copyright © 2006 John Wiley & Sons, Ltd. [source] Determining the Vapor Pressures of Diacetone Diperoxide (DADP) and Hexamethylene Triperoxide Diamine (HMTD)PROPELLANTS, EXPLOSIVES, PYROTECHNICS, Issue 6 2009Jimmie Abstract The vapor signature of diacetone diperoxide (DADP) and hexamethylene triperoxide diamine (HMTD) were examined by a gas chromatography (GC) headspace technique over the range of 15 to 55,°C. Parallel experiments were conducted to redetermine the vapor pressures of 2,4,6-trinitrotoluene (TNT) and triacetone triperoxide (TATP). The TNT and TATP vapor pressures were in agreement with the previously reported results. Vapor pressure of DADP was determined to be 17.7,Pa at 25,°C, which is approximately 2.6 times higher than TATP at the same temperature. The Clapeyron equation, relating vapor pressure and temperature, was LnP (Pa)=35.9,9845.1/T (K) for DADP. Heat of sublimation, calculated from the slope of the line for the Clapeyron equation, was 81.9,kJ mole,1. HMTD vapor pressure was not determined due to reduced thermal stability resulting in vapor phase decomposition products. [source] Investigation by solid-phase microextraction and gas chromatography/mass spectrometry of secondary metabolites in lichens deposited on stone monumentsRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 6 2003Francesco De Angelis Lichens are ubiquitous organisms formed by symbiotic associations of fungal hyphas and algae that also grow under often extreme environmental conditions. They produce secondary metabolites, the so-called lichen substances, whose structural characterization can give an important contribution to lichen taxonomy. Lichens are also widely employed as biomonitors of atmospheric pollution; being epiphyte organisms they tend, in fact, to accumulate exogenous compounds. Moreover, it could be questioned if the environmental stress alters their secondary metabolites production. Therefore, a new strategy for the analysis of the organic substances absorbed or metabolized by lichens has been developed. This method exploits the dry solid-phase microextraction (SPME) headspace technique coupled with gas chromatography/mass spectrometry (GC/MS). Lichens coating the stone surfaces of monuments, located in small towns between high mountains and far away from urban environments, have been investigated. In the field of cultural heritage, this study can contribute to the knowledge of the state of conservation of outdoor exposed historical monuments. Copyright © 2003 John Wiley & Sons, Ltd. [source] | ||||||||||