LAboratoire de Spectrochimie Infrarouge et Raman – UMR 8516
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Plateform analyses of traces : Equipments


The plateform « Spectrométrie par torche à plasma » of the Research Federation Michel-Eugène Chevreul is hosted within the platform « Analyse de traces » of the LASIR laboratory. The platform owns an axial view inductively coupled plasma atomic emission spectrometer (ICP-AES) Varian Vista Pro. A charge coupled device (CCD) covering a broad spectral range (from 167 to 765 nm) is used as a detector. This analytical technique is used for detection of metals in solution with detection limits down to few μg L-1.

The inductively coupled plasma mass spectrometer (ICP-MS) Varian 820-MS allows us to achieve even lower detection limits (below μg L-1) and is used for the analysis of trace and ultra-trace elements in various matrixes. The collision-reaction interface (CRI) located on the skimmer cone enables to handle polyatomic interferences.

ICP-AES, Varian, Vista Pro

ICP-MS, Varian, 820-MS

Since 2017, the platform is equipped with the latest generation of inductively coupled plasma mass spectrometer (ICP-MS, Agilent 7900) installed in a clean room. This spectrometer is dedicated to ultra-trace analyses (in the ng L-1 range). The octopole reaction system (ORS) allows us to manage spectral interferences. The ultra high matrix introduction (UHMI) technology extends the matrix tolerance through uses an additional argon gas flow, added between the spray chamber and the torch, to dilute the aerosol. This ICP-MS can also be coupled to liquid (HPLC Agilent 1260 Bio-Inert) or gas (GC Agilent 7890B) chromatographic systems to tackle speciation notions.

ICP-MS, Agilent, 7900 + HPLC & GC coupling

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Two mass spectrometers coupled to gas chromatography systems (GC-MS) are dedicated to the analysis of organic micropollutants such as PAHs, PCB, some pesticides and drug residues. The technical equipment consists of a Thermo ISQ-LT single quadrupole coupled to a Thermo Trace 1300 GC, and of one Varian Saturn ion trap coupled to Varian 3900 gas chromatograph. The latter is notably used for the analysis of complex organic extracts by working in the MS/MS mode.

GC-MS, Varian Saturn

GC-MS, Thermo ISQ-LT

A high performance liquid chromatography (HPLC) system Agilent 1260 equipped with both a UV diode array detector and a fluorescence detector has been installed on December 2016. This system is used for the analysis of various organic compounds as well as for the study and the characterization of organic matter through size exclusion chromatography applications.

ICS5000/3000, Thermo/Dionex

An ion chromatography system (ThermoScientific/Dionex, ICS5000/ICS3000) equipped with an eluent generator and a conductivity detector is dedicated to the analysis of anions in solution.

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Mercury analysis

Advanced Mercury Analyzer (AMA 254, from Altec Ltd., Czech Republic) is dedicated to direct total mercury analysis by atomic absorption spectrometry without any pre-treatment of the samples. Briefly the method is based on the dry decomposition of liquid or solid sample in a stream of oxygen and passage of the combustion gases through the catalytic column, followed by trapping Hg° on the gold amalgamator. Heating the amalgamator rapidly evaporates preconcentrated mercury; which is then transported into the system of measuring cells, and atomic absorption of free mercury atoms is measured. The whole analysis is performed automatically without the need of preliminary dissolution and/or decomposition of the sample. Instrument has a good sensitivity (detection limit 0,01 ng Hg), reproductibility (< 1,5%) and reliability of operation. Working range is 0,05 to 500 ng Hg.

Methylmercury can be determined, by aqueous ethylation followed by Headspace (HS) injection, Gas Chromatography separation (Clarus 500, PerkinElmer), and detection by Atomic Fluorescence Spectroscopy (Tekran, Model 2600 CVAFS Mercury Analysis System). Briefly, the extraction from 100-200 mg sediment is performed in glass vial with CH2Cl2, the mixture is shaken for 45 minutes, centrifuged for 15 min at 3000 g. After separation of the organic, aqueous phase, from solid layers, 5 mL of the organic phase is transferred to a conical glass bottle containing Milli-Q water. Back-extraction of the organic layer in the water phase is performed by solvent evaporation under constant nitrogen flow. The aqueous phase is transferred to Headspace vials. Finally, the ethylation is performed using tetraethyl borate. The detection limit of HS-GC-CVAFS is 1 ng/kg.

Système de spéciation du mercure mis en place au laboratoire

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The electrochemical techniques such as the voltammetry or the chronopotentiometry allow in much of the cases to detect in routine trace metal concentrations in the nM-µM range in aquatic systems and to perform speciation studies. Additionally, these sensitive analytical tools are compact and do not use a lot or energy, so that they can relatively easily be deployed in the field to monitor on line trace metals. A partnership with the French Water Agency Artois-Picardie has been initiated for 10 years to install our voltammetric apparatus in their mobile monitoring stations.

The electrochemical tools belonging to the Trace Analyses platform are:

• 1 potentiostat-galvanostat Autolab (Eco Chemie) ;
• 1 potentiostat-galvanostat Autolab (Eco Chemie);
• 1 potentiostat-galvanostat µAutolab type II;
• 1 portable potentiostat-galvanostat Palmsens;
• 1 Metrohm stand 663 VA with its IME 663 (Eco Chemie) to control the functioning of the mercury drop electrode;
• 1 ATMS (Automatic Trace metal Monitoring System) designed and manufactured in the laboratory with 1 potentiostat-galvanostat µAutolab type III, 1 Metrohm stand 663 VA with its IME (Eco Chemie), 3 peristaltic pumps and 3 micro-burettes and a computer to monitor the whole system.

Automatic monitoring station belonging to the French Water Agency for watching on line the water quality. The ATMS is present at the back of this station.

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