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Headspace sampling of fragranced products

Equilibrium and dynamic headspace sampling

Lotion and flowersHeadspace sampling is used widely in the food & fragrance industries. It is often employed alongside other techniques such as purge & trap, solvent extraction and SPME, in order to provide qualitative and quantitative analysis of VOCs in a sample.

Headspace techniques can be divided into two categories:

  • Equilibrium (static) headspace is a convenient sampling technique for many samples, but in cases where there is a wide range of volatiles present in a sample it is difficult to optimise the equilibration temperature.

  • Dynamic headspace sampling is a more versatile option, because it more efficiently extracts the less volatile components, leading to the generation of more comprehensive sample information in a single analysis.

What Markes can offer

Markes offers three approaches for carrying out headspace analysis, as described below.

Microchamber technologies for dynamic headspace analysis

Markes’ Micro-Chamber/Thermal Extractor uses the principles of dynamic headspace sampling to collect vapours released from a wide range of sample types.

The sample is placed in one of the compact chambers, which is held at a specified temperature as a flow of gas is applied. Analytes are collected onto a sorbent-packed TD tube for analysis by TD–GC.

A benefit of this approach is the minimal sample preparation and the rapid processing – up to six samples can be collected per hour.

Stepwise dynamic headspace analysis

Markes’ HS5-TD system enables ‘stepwise’ dynamic headspace sampling directly from standard headspace vials into the focusing trap of the UNITY thermal desorber. This multi-stage process allows extraction of a wider range of volatiles in a single run than conventional static headspace, thus generating more information from a single run.

Direct desorption

Direct desorption, a variation on the principle of dynamic headspace, is useful to understand the overall volatile content of a sample, and in some cases can achieve exhaustive extraction of the volatiles from a small sample.

Small samples of solids or semi-solids are weighed directly into empty TD tubes or tube liners. They are then heated in a stream of inert gas to sweep volatiles from the sample matrix onto the focusing trap of the thermal desorber, for analysis by GC in the usual manner.

Applications include the odour profiling and quality control of a range of relatively homogeneous materials, such as waxes, powders or pastes.

Dynamic headspace sampling

Dynamic headspace sampling, for example using micro-scale chambers such as Markes’ Micro-Chamber/Thermal Extractor, is an increasingly popular and versatile alternative to equilibrium (static) headspace, because of its ability to extract a wider range of analytes.

Continuous removal of the vapours from the sample chamber means that the sample–vapour equilibrium is constantly being re-established, leading to a greater proportion of the less volatile components being released into the headspace, and consequently the generation of more comprehensive sample information in a single run.

The size of the individual microchambers also makes this approach valuable for odour-profiling less homogeneous samples otherwise suitable for direct desorption.

Like direct desorption, raising the temperature of the sample speeds up the release of volatiles and allows the extraction of a meaningful aroma profile in a short space of time.

Further information

  • For an example of the use of direct desorption and TargetView to analyse a complex ‘betel nut’ fragranced foodstuff, see Application Note 098.

  • For examples of the analysis of fragrance profiles from...
    ...tobacco using Markes’ HS5-TD headspace system, see Application Note 096.
    ...incense sticks using Markes’ Micro-Chamber/Thermal Extractor, see Application Note 100.

  • For more examples of the use of TD-based methods for the analysis of fragrance profiles of consumer products, see Application Note 052, or contact us to obtain a copy of our TD Applications Guide on food, flavour, fragrance and odour profiling.
UK
UK
Markes International Ltd
Gwaun Elai Medi-Science Campus
Llantrisant
RCT
CF72 8XL, UK
Tel: +44 (0)1443 230935
Germany
Germany
Markes International GmbH
Schleussnerstrasse 42
D-63263 Neu-Isenburg
Frankfurt
Germany
Tel: +49 (0)6102 8825569
USA (West)
USA
Markes International, Inc
2355 Gold Meadow Way
Gold River
California 95670
USA
Tel: 866-483-5684 (toll-free)
Part of Schauenburg International
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