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 FTICR Mass Spectrometry Laboratory

 

Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR/MS) is a technique that is especially suited for the study of the chemistry of ion/molecule systems in the gas phase. As a result of the applied magnetic and electrical fields, it is possible to trap ions for long periods of time when compared with more conventional mass spectrometry techniques, and complex sequences of processes can be accomplished: ionization, selection, acceleration, ejection, collision, reaction and detection. The different event sequences correspond to different types of experiments in which ion structures, reactant/product sequences, kinetics and thermodynamic properties can be studied. The FT-ICR/MS technique is also a powerful analytical tool, displaying very high mass resolution and mass accuracy, and as it can be coupled to a large variety of ionisation methods, it can analyse numerous types of compounds and materials.

 

fticr

 

The FT-ICR/MS equipment at Campus, an Extrel/Finnigan FT/MS 2001-DT with a 3 Tesla superconducting magnet and a Nd:YAG laser for desorption/ionisation, is unique in the country, was installed in October 1991 as a result of the “Ciência” Programme and is shared by Nuclear and Technological Campus (CTN), IST and FCUL. With support of the “Praxis XXI” Programme, a new instrument control and data acquisition station, and a module for quadrupolar axialisation were installed in early 1999.

The FT-ICR mass spectrometer is run by researchers from C2TN and it is mainly used for gas-phase lanthanide and actinide chemistry studies, and also in the characterisation of lanthanide and actinide compounds. Due to its analytical capabilities, it is also used for the characterisation of organic and organometallic compounds, namely through accurate mass measurements, as requested by research groups in national and foreign universities and laboratories.

 

Contacts:

Joaquim Marçalo

João Paulo Leal  blackPhone1  219946219

 Actinide Laboratory

 

 Act1    Act2

The Actinide Laboratory, with a special air circulation system, is equipped with several glove-boxes for manipulation of actinides. It was formerly used for neptunium-237 chemistry studies.

It is currently used for the manipulation of small samples of platinum alloys containing protactinium, neptunium, plutonium, americium and curium, used as targets in gas-phase chemistry studies by FTICR mass spectrometry. This Laboratory also houses the ESI+nESI+APCI-QIT mass spectrometer.

 

Contact:

Joaquim Marçalo

 Resource facilities

 

The Laboratory of Catalysis(LC) tem has access to a broad range of techniques at the Nuclear and Technological Institute. The facilities includes analytical techniques for molecular and macromolecular characterization such as NMR, FTIR, Mass Spectrometry, Elemental Analysis (C, H, N, S), Thermal Analysis (TG, DSC), X-Ray (powder and single crystal), Gas Chromatography (CG, with TCD and FID detectors), etc.

Several reactor systems are available at the LC, including pressure reactors (autoclaves) and plug-flow type reactors (Pyrex and quartz) for measurements at atmospheric pressure. Facilities for CO safety manipulation and techniques such as TPR and TPD for catalysts characterization are also installed

On line GC analysis(TCD e FID) is the main technique used to follow the catalytic reactions. Three GC are available (Agilent 4890D with TCD, Agilent 7820, with FID and Shimadzu 9A, with TCD and FID) either for reactivity studies or for thermal characterization of the catalysts (TPR, TPD of selected molecules).
Resource facilities for the synthesis of ligands and compounds under inert atmosphere, namely glove boxes, are also on hand. The LC has also access to unusual facilities for catalysts preparation such as synthesis in liquid ammonia.

 Laboratory of Catalysis

 

The Laboratory of Catalysis (LC) is engaged on fundamental and applied research in the field of f-block elements chemistry.

LabCatF1   LabCatF2

 

Research activities can be grouped in the following categories:

Synthesis and characterization of lanthanides or actinides (U, Th) binary intermetallic compounds (IC), including nano IC.

Preparation of bimetallic oxide catalysts using the intermetallic compounds as catalytic precursors, including nanobimetallic oxides.

Preparation and characterization of chloride and carbonate molten salts containing f-block elements.

Activation of methane and reactivity studies with carbon dioxide and nitrous oxide, e.g., for the synthesis of hydrocarbons or alcohols.

 

 

Cooperation - contacts

The LC is open to cooperation, including the exchange of senior researchers as well as graduate students.
If you are interested in doing your master, PhD or post-doctoral work in Catalysis, the LC will be pleased to receive you. Grants for researchers and students having obtained a diploma in Chemistry or Chemical Engineering, or an equivalent diploma or foreign qualification, can be submitted to the Portuguese Foundation for science and Technology (FCT).

 

The f-Element Chemistry Group and the Laboratory of Catalysis will be pleased to receive your.

Contact:

Joaquim Branco,  blackPhone1 +351.219946116, email: 

Research projects

The LC has been doing research in several areas. The catalytic reactions and process under investigation are based on the activation of pollutant C1 substrates such as CH4 and CO2. The LC is also engaged in partnership projects with the industry.

A brief summary of selected projects is given below.

Oxidative Coupling of Methane using f Block Element Intermetallic Compounds as Catalytic Precursors a

The main objective of this project was to study LnCu2 (Ln=La, Ce, Pr, Nd, Gd, Tm) and AnCu2 (An=Th, U) intermetallic compounds as catalyst precursors for the oxidative coupling of methane to C2 hydrocarbons (C2H6 and C2H4), with high ethylene selectivity.
a (FCT/POCTI/QUI/35394/2000), J. alloys Comp. 478 (2009) 687-693, J. Alloys Compd., 464 (2008) 399-406.

Electrochemical and selective conversion of carbon dioxide b

Partnership with OMNIDEA (AeroSpace Technology and Energy Systems) Lda., ESA supported project “Energon - Space Long Term R&D, ESA / ESTEC - OMNIDEA, Contract No. 19594 / 06 / NL / PA”. Patent: INPI, Pt-105566.
b Protocolo ITN-QIO/OMNIDEA (2000 - ...)

Coupling catalysts with non thermal plasma for the decomposition of volatile organic compounds c

Development of a catalyst – non thermal plasma system for the activation of methane and production of syngas and hydrocarbons. Partnership ITN/ISEL. Patent: INPI, Pt-105078.
c (FC/PTDC/Equ-Equ/65126/2006), J. Mol. Catal. A: Chemical 320 (2010) 47–55; J. Alloys Comp. 497 (2010) 249–258; Plasma Chemistry and Plasma Processing 31 (2011) 427-439

Chloride molten metal salts catalysts of the type potassium-lanthanide d
Study of chloride molten salts of the type potassium-lanthanide for the catalytic reduction of nitrous oxide by methane and production of hydrocarbons.
d (FCT/PTDC/QUI/72290/2006), Catalysis Communications 12 (2011) 1425-1427

CO2 mitigation and production of methanol by reforming of CH4 e
Methanol production using methane and carbon dioxide as feedstock.
e (FCT/PTDC/AAG-TEC/3324/2012 - 2015)

Increasing the Energy Efficiency of Plasma Conversion of Methane f
Syngas production and increase of energy efficiency of non-thermal plasma.
f (FCT/PTDC/FIS-PLA/2135/2012 - 2015)