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C2TN

ETN

Elemental Characterisation and Speciation using
Nuclear Analytical Techniques

 

Nuclear analytical techniques (NATs) in general and ion beam based NATs in particular, have in essence the potencial to providing much more information out of the analysed samples, than what is usually achieved using the established methods in conservative approaches. The aim of this main activity of ETN, is thus to extend NATs capacity beyond the present state-of-the-art. Exploiting usually unused approaches, developing new specialised software and new analytical methodologies are thus the major components of the work in this context. In a recent past, a beyond the state-of-the-art instrumentation was installed and two breakthrough PhD thesis were finished. At present, operationalization, validation and fine tunning of new capabilities are underway, joins exploitation for fundamental and applied research, without losing view of the original motivation that remains an important ultimate societal challenge.

 

The HRHE-PIXE facility

 
FigMiguel

 

 

The High Resolution High Energy Particle Induced X-ray Emission (HRHE-PIXE) facility installed in 2008, is one of the few, if not still the single PIXE setup in the world, able to provide PIXE X-ray spectra covering an almost 120 keV window energy (from just below 1 keV up to above the 110 keV of the 19F(p,p'γ)19F nuclear reaction γ ray), while presenting a state-of-the-art relative resolution reaching 0.25% and always better than 1.5%.

 

 

The full 120 keV range is achieved using two detectors. A CdTe detector, operational for energies above 3.3 keV, complements a first generation transition edge sensor, TES, X ray Microcalorimeter Spectrometer (XMS), capable of providing better than 1% relative resolution from below 1.0 keV up to 20 keV, while reaching 0.25% relative resolution at 10.550 keV Pb Kα



 

 
 
 
Fundamental research

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UO2 ThickSample w300

 

The specific characteristics of the HRHE-PIXE system open the possibility to carry out fundamental research on the improvement of atomic parameters database, a very important subject presently in discussion in the frame of the X-ray Spectrometry comunity.


Allowing the separation of close laying M lines of heavy elements at the same time as being able to detect the L and K spectra, sets the possibility to use self-consistent approaches to study line intensity ratios and to reduce the uncertainty in transition energies values. 



 

Software and capacity building


DT2 interface and tails and cross secFrontier research on NATs implies developing new software, which requires among others additional developments on:


Cross-section routines:
quantifying K, L and M shell transitions must be carried out efficiently, therefore new and fast algorithms were established and included in the specific software under development, as well as integrated in the Geant4 Colaboration code.


CdTe detector response functions:
while Si(Li) detectors response function is fenomenologically well established, CdTe and other detectors, are not. Proper response functions were modelled and implemented in the dedicated DT2 code under development.

 

Applied research


MCZ recortado plus spectIn the frame of applied research, fields of intervention cover a wide scope that includes:


Mineral resources:
mappings of nearly pristine mineral samples are obtainable and the resolution allows Rare Earth Elements (REE) determination in iron (Fe) containing matrix samples.


Thin films:
the high sensitivity of ion beam NATs allows the measurement of low mass samples, while the high resolution allows the quantification of nearby elements, like Co in a TbFe film.


Nanoparticles and airborne particles:
while the picogram absolute detection limits of PIXE allow the characterisation of nanoparticle samples even when very small sample volume is available, the high throughput of the technique can be used in aerosol studies.

 

 

 

Societal challenges

Nanotoxicology and environmental health:

Cl vs diabetes 2009

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a decade ago, the quest for elemental speciation using NATs was a response to the need to identify chemical species of airborne elements. The LCEA laboratory installation in 2008 and the identification, in 2009, of a relation between airborne chlorine in PM2.5 and diabetes incidence, were two important marks in this quest. The ultimate goal was not yet achieved, but possible ways there are being pointed out.

 Luminescence dating laboratory

 

PictureL1 

 

SHORT DESCRIPTION

The Luminescence Dating Laboratory makes the luminescence dating method available to the archaeological/geomorphological/ geological/art-historical communities. This method evaluates the time since crystalline minerals were exposed to light or heat: examples are of mineral grains of sand from sediment or a ceramic piece, and microcrystalline phases in an archaeological artifact manufactured from flint.

 

The method

Luminescence dating is based on a combination of retrospective dosimetry and environmental dosimetry. The normal age range for dating is between 50 years and 100 thousand years. However, depending on the dosimetric properties of the signal and material being analysed, and the radioactivity of its environment, this method is able to date exposition to sunlight or firing between 0 years and >1 million years. The materials analysed for dating are inorganic and are highly resistant to alteration during their burial. Luminescence dating is therefore optimized for studies of the chronologies of human development and environmental records during the Holocene and late Quaternary. In addition to dating per se, the Luminescence Dating Laboratory has interests in the development of new methodologies and applications related with dating; retrospective dosimetry; environmental dosimetry and radiogeochemistry; and investigation of the origins and physical processes of luminescence in minerals.

The work of the Luminescence Dating Laboratory is conducted through a combination of research projects, supervision of masters and doctoral theses, and service work to private and public entities related with cultural heritage and geosciences. If you are interested in developing a project, or in the dating or other luminescence analysis of a site or group of samples, please contact us as early as possible so that we can help to optimise sampling strategy and design of the work program to address the questions that you intend to investigate. For service work, just as in research projects, following consultation we will normally aim to perform the sampling ourselves, accompanied by the client/colleague. In this way we have the best chance of maximizing the information obtained per sample analysed.

 

AVAILABLE EQUIPMENT

Sampling and Sample Preparation


Tubes for sampling sediments in stainless steel and plastic c. 10 ml to c. 1 l.
Diamond saw, hollow diamond drills and tungsten drills, water cooled, for subsampling pieces and stones.
Hydraulic press for disaggregation.
Range of calibrated sieves (63 m - 2 mm) for grain-size separation (< 90 m settled in water or acetone).
Centrifuge (4x500ml or 8x50ml), temperature controlled and ventilated with filtering of gasses.
HF rated fume cupboard, ventilated with filtering of gasses.
Heavy liquid (LST Fastfloat) for density separation to c. 3 g/cm3.
Range of strong acids for dissolution of mineral phases (ex. HCl, HF, Fluorosilicic).
Stainless steel and aluminium disks, 1 cm diameter and for single grains, for presentation of prepared fractions for luminescence measurement.
Ovens for thermal treatments to 1200°C.
High precision balance.
Binocular microscope.
Magnetic separator

  PictureL2  PictureL3a
 PictureL3b

 

Luminescence Analysis


Three Risø DA-20 automatic readers with Beta irradiator, 90Sr/90Y plaque (40mCi@2007) in calibrated geometry, and photomultiplier for detection between 160 and 630 nm:
-> aliquots measured by TL, and OSL stimulated with LEDs (c. 470 nm, c. 875 nm);
->one of them ables for single grains measured by OSL stimulated by laser/laser diode (532 nm, 830 nm);
Daybreak Beta irradiator, 90Sr/90Y plaque (40mCi@2000) in calibrated geometry.
Littlemore Alpha irradiator with vacuum system, 241Am foils (total 182mCi@2001) in calibrated geometry.
Range of glass filters for choice of detection band (or stimulation band from halogen lamp).

 

PictureL4  PictureL5

Risø Automatc Reader DA-20

 

PictureL6

Irradiador Daybreak Beta.

 

Dosimetric Analysis


In situ gamma spectrometry with calibration for sediment dosimetry based on measurements in the "Oxford blocks":
-> Osprey Universal Digital MCA Tube Base for Scintillation Spectrometry, with NaI probe, 2"x2";
-> 2 x HPI Rainbow MCA with NaI probes, 1"x1", 2"x2" e 3"x3".

 

PictureL7

 Gamma spectrometers and NaI probes for in situ measurements

 

 

Further information:


M. Isabel Dias ().   blackPhone1 +351-21-9946222 

Ana Luisa Rodrigues ().   blackPhone1 +351-21-9946224

e-mail:  

 

 

 

 

Air Quality Laboratory

 

The Air Quality Laboratory is equipped with instruments for evaluating

the ambient air quality

meteorological stations and samplers to collect particles with different size ranges, in different matrixes, in a simple or sequential way;

  • Gent samplers -  simultaneous sampling of PM5 and PM2.5-10
  • Partisol 2000 – Thermo Scientific – sampling of PM10 or PM5
  • Sven Leckel samplers to collect PM10 and PM5

the indoor air quality

equipment to monitor gases such as carbon monoxide, carbon dioxide, volatile organic compounds, ozone, formaldehyde and PM mass and number concentrations;

  • Dust Track DRX 8533 - simultaneous and online measurement of PM10, PM5, PM5, PM1
  • Particle counter 10nm-1um TSI 3007
  • Graywolf -  Wolfsense Solutions – simultaneous and online measurement of VOC, CO, CO2 and O3
  • Formaldemether htV-m – online measurements of CH2O

 

exposure

personal equipment to measure exposure to particles and black carbon and GPS.

  • Sioutas Personal Cascade Impactor (simultaneous sampling of PM25, PM0.25-0.5, PM0.5-1,PM1-2.5)
  • PM5 and PM10 Impactor PEMTM (sampling of PM2.5 and PM10)
  • Pumps Leland Legacy
  • Defender Calibrator (BIOS)
  • Micro Aethalometer AE51

 

MA3 MA1  MA2

 

PictureMA4

Participation of NET aerosol samplers in an inter-comparison exercise organized by IAEA in NCSR-Demokritos, Greece.

 

Contact Person: Marta Almeida

Email:

blackPhone1  219946124

 

Laboratories for Instrumental Neutron Activation Analysis

 

Thirty four elements commonly found in environmental and biological samples -  Al, Ca, Cu, Mn, Ti, V, As, Ba, Br, K, La, Na, U, Ag, Cd, Ce, Co, Cr, Cs, Eu, Fe, Hf, Hg, Rb, Sb, Sc, Se, Sm, Sr, Ta, Tb, Th, Yb and Zn are determined by Instrumental Neutron Activation Analysis using the k0 method (k0-INAA) that was established at the Portuguese Research Reactor (RPI).

 

PictureMA1

The elements from Al to V that produce short-lived nuclides are analyzed by a short irradiation on SIPRA - a Fast Pneumatic Sample Transfer System - and then counted on a coupled Ge detector.

  

PictureMA2

The elements from As to Zn that produce medium and long lived nuclides are analyzed by a long time irradiation at Cell55 or Cell56 of the RPI and then measured on Ge detectors associated with automatic sample changers

 

  

PictureMA3

A Compton Suppression System (CSS) is available to improve the detection limits of specific elements.

  

Equipment

4 Germanium detectors

3 DSPEC Jr 2.0

1 DSPEC PRO

2 Automatic Sample Changers

Compton Suppression System

Fast Pneumatic Transfer System

 

 

Equipment partially funded by Fundação para a Ciência e Tecnologia – National Plan for Scientific Re-equipment  REEQ/1075/FIS/2005

 

Contact Person: Marta Almeida

Email:

blackPhone1  219946124

 Instrumental Neutron Activation Analysis Laboratories - Comparative Method

 

Nuclear radiation produced by activated products is measured by high-resolution gamma spectrometers, including high purity germanium detectors coupled to pre-amplifiers, amplifiers and multichannel analysers.


The comparative instrumental neutron activation analysis method of CTN/IST allows the determination of 30 chemical elements (Na, K, Fe, Sc, Mn, Cr, Co, Zn, Ga, As, Br, Rb, Zr, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Lu, Hf, Ta, W, Th and U) with high precision and accuracy in geologic, environmental and biological samples, in samples from cultural heritage (archaeological ceramic and raw materials, monuments stones, outcrops of potential raw material, etc). Besides, it’s also determined by INAA the Au contents (in sediment samples) and Cu, Ge, Ni, Ir and Au (in meteorites). Some synthetic materials (like glass or polyethylene) are also analyzed in INAA laboratory.

 

Equipment available in the gamma spectrometry laboratory:


• Four high purity Ge detectors:
      - 3 of high energy (CANBERRA GC3019 – 5Kv; GC4018 – 3Kv; GC3518 – 3Kv)
      - 1 of low energy (CANBERRA GL3825L – 4Kv)
• Two amplifiers – CANBERRA 2020
• Two amplifiers – CANBERRA 2022
• One amplifier CANBERRA 2026
• Two high tension sources – ORTEC 459 (0 – 5Kv)
• One high tension source – ORTEC 659 (0 – 5Kv)
• Two high tension sources – CANBERRA 3106D (0 – 5Kv)

Picture1

Panoramic view of one of the gamma spectrometry laboratory

 

• Sample Changer Gamma Analyst:

      - 1 integrated system DSA 2000/A CANBERRA 3106 (0-5 Kv)
      - 1 CANBERRA detector BE 3830 – 5 Kv

Picture2a  Picture2b

Picture2c

Gamma spectrometer with a high purity Ge detector and a automatic sample changer (Gamma Analyst - CANBERRA)*

 

* Equipment funded by FCT – Fundação para a Ciência e a Tecnologia - National Plan for Scientific Re-equipment (Plano Nacional de Re-equipamento Científico). Project: REEQ/590/CTE/2005. 

 

Equipment access: 

Available for the scientific community.

 

Researcher responsible for the laboratories: 

Maria Isabel Prudêncio

 Contacts:

Maria Isabel Prudêncio ()

                  Rosa Marques ()