Workshop on thermal desorption & other miniaturized techniques - September, 18, 2017


Measurement of Air quality & material emissions: the key role of Thermal Desorption sampling.

Catherine Brasseur
Certech, Belgium


Thermal desorption sampling refers to a wide variety of sampling configurations, depending on the application. The evolution of the technique from single-stage to two-stages thermal desorption has extended the range of applications, improving the sensitivity and the possibilities from exploratory studies to final monitoring.

In this tutorial, the different steps and techniques to ensure the monitoring of air quality and material emissions will be reviewed, from conditioning and sampling to analysis. Applications will be presented, focusing on environmental and workplace monitoring, construction material emissions, odor profiling as well as automotive market requirements.


New developments in thermal desorption for air analysis and fully automated material emissions analysis.

Yunyun Nie
Gerstel GmbH, Germany


Thermal extraction combined with GC/MS is a well-established method for the determination of VOCs and SVOCs from materials used indoors and in vehicles. Unlike solvent extraction methods, thermal extraction does not reach equilibrium. The quality of results depends strongly on: temperature, time, gas flow and sample preparation. This presentation focuses mainly on the influence of temperature and on new ways to validate it for quality control purposes. Micro-scale chamber methods up to 1L volume are frequently used for screening of emissions from materials. An automated solution for sampling and determination of VOCs and of airborne aldehydes (DNPH) will be presented. Finally, a new method based on online sampling and derivatization of formaldehyde on TenaxTA will be presen-ted, showing the use of thermal desorption GC/MS for the determination of Formaldehyde. Examples shown are: PP granulate, PU foam, leather, paint, carpet, wood products, and e-cigarette liquids.


Application of thermal desorption to the analysis of semi-volatile organic compounds in indoor airborne particles.

Fabien Mercier
LERES, France


People are exposed to multiple pollutants, especially indoors. In the perspective of a cumulative risk assessment, a multi-residue method was developed for the simultaneous analysis in airborne particles of several classes of semi-volatile organic compounds (SVOCs), from trace to highly concentrated compounds. The method was based on gas chromatography/tandem mass spectrometry (GC/MS/MS) and thermal desorption (TD), a suitable on-line alternative to traditional off-line extraction techniques that require relatively large amounts of sample and organic solvent, and generally involve tedious and time-consuming multi-step procedures. This TD-GC/MS/MS method is simple and efficient. It provides many advantages over traditional methods including organic solvent-free, reduced analysis time and cost, and high sample throughput, making it appropriate for environmental monitoring programs or large-scale studies.


Thermal Desorption-Comprehensive GC link to high resolution mass spectrometry (TD-GCxGC- (HR)-TOF-MS) for to biological application.

Jean-François Focant
Department of Chemistry, Liège University, Belgium


Efficient trapping, separation, and identification of volatile organic compounds (VOCs) produced during complex biological processes require the use of multi-dimensional techniques such as TD-GCxGC-(HR)-TOF-MS.  We currently use it to create large matrices of data that are further processed to statistically differentiate between classes of samples in several medical and forensic applications.


Evaluation and Application of SPME Arrows.

Jason Herrington
Restek Corp, USA


Solid phase microextraction (SPME) fibers were developed/patented by Janusz Pawliszyn in 1990 and subsequently licensed to Supeclo until 2014. Consequently, SPME technology has largely remained unchanged over the last 26 years and is subject to following significant drawbacks: limited mechanical stability and small phase volumes. The PAL SPME Arrow was developed to overcome the aforementioned shortcomings. SPME Arrows have an outer diameter of 1.1mm. Compared to traditional SPME fiber diameters of ~0.5 mm, SPME Arrows have relatively larger sorption phase surfaces (up to 6x) and volumes (up to 20x as shown in figure below). In addition, the arrow-shaped tip facilitates smooth penetration of vial and injector septa, and the Arrow design fully protects the fiber, thereby minimizing adverse influences and loss of analytes during transfer processes. The following presentation will provide an evaluation of PAL SPME Arrows and side-by-side comparison with traditional SPME fibers. An application to ISO 17943, which capitalizes on the claimed advantages of SPME Arrows will be presented as well.


Workshop SBSE - September, 19, 2017


From sorption to SBSE/HSSE: a long history in the analysis of the volatile fraction of natural products and food.

Carlo Bicchi
Laboratory of Pharmaceutical Biology and Food Chemistry, Italy


Sorption is a concentration approach for sample preparation that has only recently become really popular. The first applications to natural products and food dated the beginning of the eighties; since then, sorption has enjoyed a continuous development. This presentation discusses the contribution of sorptive techniques to the evolution of sample preparation also in view of the development of Total Analysis Systems (i.e. TAS). The sorption achievements will be illustrated with some examples in different fields going from the first experiments with open tubular traps (OTT) to high concentration capacity techniques such as SBSE, HSSE, STE (sorptive tape extraction) and SE-HSSE (Solvent Enhanced-Headspace Sorptive Extraction) illustrates.


ICE Concentration Linked with Extractive Stir bar (ICECLES): A novel sample preparation technique for ultratrace analysis.

Brian A. Logue, Nujud Maslamani, Abdullah Alluhayb, Joseph Dzisam, and Erica Manandhar


The ability to determine contaminants at “ultratrace” concentrations is a critically important, but currently challenging, aspect of many types of analyses, including ensuring safe drinking water. Our recently discovered technique, coined ICE Concentration Linked with Extractive Stir bar (ICECLES), is a significant step towards routine ultratrace analysis. ICECLES combines the highly complementary techniques of stir bar sorptive extraction (SBSE) and a little-known concentration technique called freeze concentration (FC). During ICECLES, solutes are concentrated in the liquid solution remaining as a sample is frozen and stirred vigorously with a sorbent-coated stir bar. Currently, ICECLES has produced pg/L limits of detection and up to 1000-fold signal increases compared to SBSE. We will give an overview of ICECLES and show its excellent applicability for ultratrace analysis and food/flavor investigation.


Coupling SBSE to the Direct Analysis in Real Time (DART)/ high resolution mass spectrometry (HRMS) : some applications.

Maxime Bridoux
Commissariat à l’Energie Atomique et aux Energies Alternatives, France


Mining companies producing uranium are subject to strong environmental regulations aimed at reducing the impact of their sites on the environment. In this industrial and supervisory context, this work focused on the development of a rapid quantitative analysis method, including an in-situ sampling step for extractants entering the nuclear fuel cycle.

In order to be consistent with an objective of environmental compliance, and taking into account the new techniques available, a solventless extraction technique has been chosen, in accordance with the precepts of a more "green" chemistry, combined with an Analytical technique based on the coupling of a DART (Direct Analysis in Real Time) ionization source to high resolution mass spectrometry (LTQ Orbitrap XL ™).

The sampling technique chosen was the polymer extraction deposited on a magnetic stirring rod, more generally known under the acronym "SBSE" (Stir Bar Sorptive Extraction). Once the analytes are extracted from the matrix by the SBSE bar (called Twister ™), the one is positioned in the helium atoms stream excited and heated to 300 ° C. The metastable helium atoms (He *) are then projected onto the polymer having extracted the analytes and cause both the vaporization of the analytes and their ionization by energy transfer.

The strengths of the method developed are the quasi-instantaneous identification of the analytes by high resolution mass spectrometry (Orbitrap) as well as their quantification by means of an isotopic dilution. This provides a simple and economical alternative to spot sampling to obtain a realistic estimate of the contamination of surface and ground water by organic micropollutants. These solventless and chemical-free procedures are particularly suited to operational applications requiring minimal logistics and transport constraints.


A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique for enhanced recovery of polar solutes in aqueous samples.

Nobuo Ochaiai
Gerstel K.K., Japan


A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique was developed for enhanced recovery of polar solutes in aqueous samples. A conventional PDMS stir bar was swollen in several solvents with log Kow ranging from 1.0 to 2.0 prior to extraction. After extraction, thermal desorption – gas chromatography – (tandem) mass spectrometry (TD-GC-(MS/)MS) or liquid desorption – large volume injection (LD-LVI)-GC–MS were performed. Compared to conventional SBSE, SA-SBSE using diethyl ether, dichloromethane, and diisopropyl ether provided higher extraction efficiency from aqueous samples for solutes with log Kow< 2.0. The performance of the SA-SBSE method is illustrated with analyses of aroma compounds in beverages and of pesticides in wine.


Octopus : finding sources of pollutions in sewage networks.

Christophe Tondelier
Veolia Research & Innovation, France


Octopus is a silicone based integrative sampler adapted to wastewater networks. Octopus allows the capture of organic contaminants in this miscellaneous environment. It is used in support of police actions in the networks aiming for the localization of the sources of contaminations of the waste water witch lead to non-compliance on sludge and treated wastewater.


The contributions of SBSE and thermo-desorption for contaminants monitoring in cooperage.

Bertrand Leaute
Laboratoire d’Expertises Conseils,


The aging of wines in barrels is a luxury reserved for high value-added wines, the monitoring of contaminants like HaloAnisoles & HaloPhénols type has become a major challenge for coopers.

The sensitivity and versatility of the SBSE and the TD-GCMS have enabled the LEC to develop effective approaches to meet the sector's specific expectations, ranging from the analysis of the raw material to the validation of the finished product.

SBSE applied to evaluate personal protective equipment against NBC threats.

Gilles Richner
Spiez Laboratory, Switzerland


First responders and soldiers should be able to perform their duty under the safest working conditions even when operating in chemically contaminated environments or under NRBC threats. The efficiency of NRBC individual protection equipment (IPE) is assessed in a test chamber simulating a contaminated field, where passive samplers (e.g. SBSE) are placed inside the IPE to measure the local exposure dose of the skin.


Development and validation of an analytical SBSE-GC-MS/MS method for the analysis of organic micropollutants in fresh waters. Impact of suspended solids.

Yvan Gru
GIP Inovalys, France


An analytical method using the SBSE extraction technique on magnetised bar associated with gas chromatography and tandem mass spectrometry has been developed and validated in freshwater matrices for the analysis of multi-class organic compounds (HPA, PBDE , PCBs, organochlorine pesticides, organophosphorus pesticides, etc.). A study of the impact of suspended solids (SS) was also carried out to evaluate the field of use of this method and thus to verify the potential for the extraction of SBSE regarding dissolved and particulate fractions of surface water.


New SBSE applications for Continuous Flow Integrative Sampler to analyze emerging compounds in water.

Julio Llorca
Labaqua, Spain


The analysis of spot samples it only will provide a snapshot of the concentration in the environment. Devices as passive samples and integrative systems have been developed for the monitoring of organic contaminants in aquatic environments and permits to obtain average concentration over long-term exposure.
Continuous flow integrative sampler (CFIS) using PDMS under the commercial twister format as sorbent and Thermal desorption as analytical methods have be used to determine average concentrations of non-polar emerging and priority pollutants in water samples.


Application of SBSE to the quantification of pesticides and endocrine disrupting compounds in biological fluids.

Marie-Laure Bayle
Rovaltain Research Company, France


Pesticides and endocrine disrupting compounds are known environmental contaminants. Because they are ubiquitous, living organisms may be exposed for a short or longer time. This exposition can be revealed by the analysis of specific biofluids such as urine or plasma.
This study focuses on the use of SBSE for the analysis of bisphenol A in urines and a multi-residue method for the analysis of pesticides in urines.



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