Static & Dynamic Headspace
Static & Dynamic Headspace

Headspace Analysis

For static and for dynamic headspace analysis only a dedicated tool is inserted into the PAL System and can be used immediately. Even all other tools for liquid injection or Solid Phase Micro Extraction (SPME) can still be used for additional methods without any change of the hardware making the PAL System a real multi-method device for any kind of samples and sample preparation methods for GC and GC/MS analysis.

static headspace tool

Static Headspace Analysis

The static headspace analysis (HS-GC) is the easiest method. Only little sample preparation with homogenization is required, then adding the liquid or solid sample to 10 or 20 ml headspace vials, weighing, and placing the well-capped vials into the racks of the PAL System. The PAL headspace workflow takes over and injects finally into the GC or GC/MS system.

The static headspace analysis is applicable for all analytes with significant vapor pressure. Typically, volatile organic compounds (VOCs) analytes are understood with boiling points up to 250°C, covering analytes of natural and anthropogenic sources. The United States EPA method 5021A lists more than 70 compounds, mainly solvents of environmental importance, that are included in this standard method [1].
 

ITEX-DHS tool

Dynamic Headspace Analysis ITEX DHS

The dynamic headspace analysis (DHS) with the ITEX DHS Tool extends the range of analytes to those with lower vapor pressure and higher boiling points.

In contrast to the static headspace method, which uses an equilibrium between the sample and the headspace above, the dynamic method is an exhaustive procedure. The analytes of interest are continuously driven out of the sample and collected on the ITEX trap until analysis.

Only the PAL System runs static and dynamic methods on one and the same instrument. Previous instrumental solutions required two dedicated and space-consuming equipment.

A variety of sorbent materials are available comprising the standard Tenax TA/GR, and as well Carbopack, Carboxen and Carbosieve sorbents.

ITEX enrichment procedure

ITEX DHS offers the dynamic headspace enrichement of volatile & semi-volatile compounds from solid, liquid and gaseous samples. The sorbent material is embedded in the upper part of a syringe needle. This analyte trap is temperature controlled by an integrated cooling fan and the trap flash heater for a quick desorption into GC.

ITEX DHS Sampling

Effective Extraction with Purge Strokes

References

[1] U.S. EPA, 2014. Method 5021A. Volatile Organic Compounds in Various Sample Matrices using Equilibrium Headspace Analysis. SW-846 Update V, Rev.2.

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Extraction of volatile compounds is a widely used approach for analysis of foods and beverages.  By the nature of gas phase sampling, the limiting factor for polar analytes are given by low vapor pressure or higher boiling points of semi-volatile compounds. These limitations can be overcome by sampling at decreased pressure levels using vacuum conditions. This has been shown in several publications using vacuum sampling techniques. In this study, a fully automated approach of Vacuum In-Tube Extraction (V-ITEX) is presented, a simple and fully automated technique using PAL system autosamplers. The application examples include flavors, fragrances, off-flavors, pesticides and biomarkers by extractions directly from the food sample matrix, such as Honey, Bee Wax, Cheese, Onions, Blood and Urine.  

Presented by:

Pascal Fuchsmann, Head of Flavor Analytics Agroscope

Stefan Cretnik, Product Manager CTC Analytics AG

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