joint research centre (jrc) - cea/cea

SEMINAIRE CETAMA May 2011 – Event Name 1

IRMM - Institute for Reference Materials and MeasurementsGeel - Belgium

http://irmm.jrc.ec.europa.eu/http://www.jrc.ec.europa.eu/

Joint Research Centre (JRC)

50 years of successful cooperationIRMM - CETAMA

SEMINAIRE CETAMA May 2011 – Montpellier_France 2

Founders

New ideas for lasting peace and prosperity…

Konrad Adenauer

Robert Schuman

Winston Churchill

Alcide De Gasperi

Jean Monnet


The treaties – basis for democratic cooperation

1952 The European Steel and Coal Community

1958 The treaties of Rome:

The European Economic CommunityThe European Atomic Energy Community

(EURATOM)

1987 The European Single Act: the

Single Market

1993 Treaty of European Union

– Maastricht1999

Treaty of Amsterdam2003

Treaty of Nice


25 March 1957 - The Treaty of RomeEuropean Economic Community and EuratomBirth of the CommissionCreation of the JRC

Legal basis: the European Atomic Energy Community Treaty – Article 8

‘The Commission […] establishes a Joint Nuclear Research Centre. The Centre ensures that research programmes and other tasks assigned to it by the Commission are carried out.... For geographical or functional reasons, the activities of the Centre might necessitate separate establishments ...’

The past


Where does the JRC fitin the European Commission?

Commissioner Geoghegan-QuinnResearch, Innovation and Science

Joint Research Centre (JRC)

President Barroso 27 Commission Members

Research DG (RTD)

The present

Director general D Ristori

http://ec.europa.eu/commission_2010-2014/geoghegan-quinn/index_en.htm


7 Institutes in 5 Member States

IRMM -

Geel, BelgiumInstitute for Reference Materials and MeasurementsITU -

Karlsruhe, GermanyInstitute for Transuranium

Elements

IE –

Petten and Ispra, The Netherlands and ItalyInstitute for Energy

IPSC -

Ispra, ItalyInstitute for the Protection and Security of the Citizen

IES -

Ispra, ItalyInstitute for Environment and Sustainability

IHCP -

Ispra, ItalyInstitute for Health and Consumer Protection

IPTS -

Seville, SpainInstitute for Prospective Technological Studies

The present


Euratom Treaty - Central Bureau for Nuclear MeasurementsMission defined: ‘A bureau of Standards specialising in Nuclear Measurements for Isotope Analysis and Absolute Measurement of Radiation and Neutron Absorption’Central Bureau for Nuclear Measurements was established in Geel

1962 Van de Graaff accelerator installed1963 first on-site mass spectrometry1965 LINAC inaugurated

Mandate extended to other fields & policies e.g. industry, food safety, environmental pollution, customs and trade

developping and disseminating measurementstandards (reference materials)1993 Renamed ⇒ IRMM Institute for Reference Materials and Measurements

The past


The mission of the IRMM is to promote a common

and reliable European measurement system

in support of EU policies.

IRMM - CONFIDENCE IN MEASUREMENTS®

The present


50th anniversary of IRMM Symposium on the Future of

Reference Materials – Science and Innovation

23-25 November 2010 at IRMM

in Geel, Belgium

The past

CETAMA GT 03 « analyse du plutonium »working group meeting

8-9 February 2010 at IRMM, Geel, Belgium


50th anniversary of CETAMA SEMINAIRE CETAMA

ANALYSES ET MESURES POUR LE NUCLEAIRE :

LES ENJEUX ET LES TENDANCES FUTURES

24 AU 26 MAI 2011LE CORUM – MONTPELLIER

The present

Sa mission principale est de promouvoir les bonnes pratiques analytiques et de faire partager les connaissances et savoir

faire acquis dans les différents laboratoires


The prime objective of JRC-IRMM is…

… to build confidence in measurements and ensuring their comparability

•

Method development and validation•

Reference measurements (ISO17025)

•

Reference materials (ISO34)•

Inter-laboratory comparisons (ISO17043)

•

Training materials•

Validated data


… to implement best practice and knowledge transfer•

Thematic networking

•

Method development and validation•

Reference measurements

•

Production and disseminationof reference Inter-laboratory comparisons

•

Seminars, summer schools

Objectives of CETAMA


CETAMA – IRMM throughout the years

1)

Provison

of CETAMA reference

materials

(RMs) to IRMM2)

Development of RMs

and interlaboratory

comparison test samples

3)

IRMM invited by CETAMA to join CETAMA GT 03 «

analyse du plutonium »

4)

Participation of IRMM in EQRAIN, CEA labs in REIMEP/NUSIMEP5)

Production and certification of Pu metal

reference

material

MP2

6)

IRMM participation in CETAMA GT 12 «

spectrométrie de masse

»7)

CETAMA GT 03 working

group meeting held

at

IRMM in 2010

8)

Sharing other

platforms

(ESARDA WG DA, IAEA CGM, CEA/DAM-JRC)


Les enjeux - challenges

•

Support nuclear safeguards and fissile material control by providing metrological tools for bulk and particle analysis

•

Reference materials to the highest standard of uranium and plutonium also for measurements of environmental samples

Uranium oxide reference particles

Large Sized Dried Spikes

LSD

Uranium isotopic RM



•

New spike RMs for IDMS

•

Stability and shelf-life of Pu, U RMs

•

RMs for “age dating”

•

Development of Uranium Reference Particles

•

Advancements in mass spectrometry technqiues for nuclear material and environmental sample analysis

•

External quality control tools (ILCs)

•

State-of-the-practice performance criteria (ITVs)


Modified Total Evaporation (MTE) • New tool for TIMS for measurements of U-minors in nuclear

safeguards; forensics; geo-and cosmo-chemistry; • unprecedented level of accuracy for isotope ratio measurements; • joint advancement in measurement sciences of international reference

and safeguards laboratories (IRMM, ITU, NBL, IAEA-SGAS)

Journal of Analytical Atomic Spectrometry, 2011, 26, 550



Metal Plate: Wirtz Metal Cube: Heisenberg

Plate (Mass%) Cube (Mass%)

234U 0.005 35 (10) 0.005 30 (9)

235U 0.710 9 (8) 0.710 9 (8)

238U 99.283 7 (21) 99.283 8 (10)

Same source

material ?

Nuclear forensics – uranium minor isotopes



Isotopic “fingerprinting”• Detection of any undeclared nuclear material or activities

– Nuclear safeguards• Attribution of intercepted materials

– Nuclear forensics• Response to theft, illegal transfer of nuclear materials

– Nuclear security

1 um particle of U

1

10

100

1000

10000

100000

0 10 20 30 40 50 60Age [years]

Num

ber o

f Th-

230

atom

s

0.7%5%50%93%

6.3395E-03

6.4804E-03

6.6213E-03

6.7621E-03

6.9030E-03

7.0439E-03

7.1848E-03

7.3257E-03

7.4665E-03

7.6074E-03

7.7483E-03

1772

1830

1759

1756

2111

1767

1768

1758

1750

1753

2110

1850

1757

1752

1754

1749

1755

1751

1766

1770

n(23

5 U)/n

(238 U

)

-10

-8

-6

-4

-2

0

2

4

6

8

10

Devia

tion

fro

m t

he c

ert

ifie

d v

alu

e [

%]

n (235U)/n (238U)

NUSIMEP-6: Uranium isotope amount ratios in uranium particles Certified value for n (235U)/n (238U) : 0.007 043 9 ± 0.000 003 5 [U=k·u c (k=2) ]

This graph displays all measurement results and their associated uncertainties.These uncertainties are shown as reported, with various coverage factors and levels of confidence.The grey band represents the reference interval (Xref ± 2uref).

'less than' value reported by lab 1770value > 10% reported by lab 1766 value < - 10% reported by lab 1772probable reporting error by labs 1766 and 1770

Laboratory code

±1%

6.3395E-03

6.4804E-03

6.6213E-03

6.7621E-03

6.9030E-03

7.0439E-03

7.1848E-03

7.3257E-03

7.4665E-03

7.6074E-03

7.7483E-03

1772

1830

1759

1756

2111

1767

1768

1758

1750

1753

2110

1850

1757

1752

1754

1749

1755

1751

1766

1770

n(23

5 U)/n

(238 U

)

-10

-8

-6

-4

-2

0

2

4

6

8

10

Devia

tion

fro

m t

he c

ert

ifie

d v

alu

e [

%]

n (235U)/n (238U)

NUSIMEP-6: Uranium isotope amount ratios in uranium particles Certified value for n (235U)/n (238U) : 0.007 043 9 ± 0.000 003 5 [U=k·u c (k=2) ]

This graph displays all measurement results and their associated uncertainties.These uncertainties are shown as reported, with various coverage factors and levels of confidence.The grey band represents the reference interval (Xref ± 2uref).

'less than' value reported by lab 1770value > 10% reported by lab 1766 value < - 10% reported by lab 1772probable reporting error by labs 1766 and 1770

Laboratory code

±1%

NUSIMEP-6

SIMS ANALYSIS WAS PERFORMED BY EC JRC ITU

Ion image of particles, single deposition. The particles are better defined and there is less uranium background than in the NUSIMEP sample.

NUSIMEP-6

SIMS ANALYSIS WAS PERFORMED BY EC JRC ITU

Ion image of particles, single deposition. The particles are better defined and there is less uranium background than in the NUSIMEP sample.

Age determination

Anal. Chem, 83 (2011) 3011-3016


Chernobyl samples [Jakopic et al.]

0.35

0.36

0.37

0.38

0.39

0.4

0.41

0.42

0.43

K2 K3 K5 K6 Oko13 Oko20

n(24

0 Pu)/

n(23

9 Pu)

IAEA 368

collected at Moruroa

Atoll, the former nuclear weapon testing site. Activity concentration 31 Bq/kg (239+240Pu)

IAEA 368 Radionuclides in Pacific Ocean Sediment

0.02

0.03

0.04

0.05

0.06

Jakopic et al. Muramatsu et al. Donard et al. Kim et al. Liao et al.

n(24

0 Pu)/

n(23

9 Pu)

Environmental samples from Chernobyl: K2-K6 core soil sampled 2, 3, 5 and 6 cm from the top Oko13 moss sample same sampling siteOko20 moss sample 1-2 km distance from the nuclear power plant

Isotopic plutonium ”fingerprint”

using TIMS

•Weapons-grade 240Pu/ 239Pu ~ 0.03-0.07

Isotopic plutonium ”fingerprint”

using TIMS

•Reactor-grade 240Pu/ 239Pu ~ 0.4 or higher

•Global fallout 240Pu/ 239Pu ~ 0.18

Pu – “fingerprints” in environmental samples

J. Anal. At. Spectrom., 2010, 25, 815–821


Survey on participation in envisaged REIMEP/NUSIMEP ILCs

0

10

20

30

40

50

60

REIMEP_17input s. REIMEP_19Pu REIMEP_20U REIMEP_21UF6 NUSIMEP_7Uparticles NUSIMEP_8U_or_Pu NUSIMEP_9env_s OtherNUSIMEP/REIMEP



Training, education, exchange expertise

Chapter I of the EURATOM treaty concerning the promotion of research European Council conclusion on the need for skills in the nuclear field

• ENEN training courses on safeguards– ESARDA academic course on Nuclear Safeguards and Non-Proliferation– BNEN advanced course on safeguards in Belgium

• Use of Reference Materials and the Estimation of Measurement Uncertainty

• Nuclear forensics training

• EUSECTRA -

European nuclear security training centre

Separation of mother & daughterisotopes → only mother isotope left;

“clock” set to zero↓

build up of daughter isotopes with time↓

measure mother/daughter isotope ratio↓

“age” calculation© The University of Western Australia

241Put = 241Pu0 * e-λ*t λ = t1/2-1* ln 2

241Amt = 241Pu0 - 241Put = 241Pu0 *(1 - e-λ*t)

R241Pu/241Am = 241Put / 241Amt = e-λ*t * (1 - e-λ*t)-1

t = λ-1*ln[(R241Pu/241Am+1)*R241Pu/241Am-1]

↓

Nuclear age datingSeparation of mother & daughterisotopes → only mother isotope left;

“clock” set to zero↓

build up of daughter isotopes with time↓

measure mother/daughter isotope ratio↓

“age” calculation© The University of Western Australia

241Put = 241Pu0 * e-λ*t λ = t1/2-1* ln 2

241Amt = 241Pu0 - 241Put = 241Pu0 *(1 - e-λ*t)

R241Pu/241Am = 241Put / 241Amt = e-λ*t * (1 - e-λ*t)-1

t = λ-1*ln[(R241Pu/241Am+1)*R241Pu/241Am-1]

↓

Nuclear age dating


Dedicated ESARDA WG DA workshops

Dedicated WGDA Workshop in conjunction with annual working group meeting, on Uncertainties in Nuclear Measurements at the IAEA in Vienna, 8-10 November 2011

• Uncertainty estimation from state-of-the-art to state-of-the-practice measurements

• Investigation of major contributions to the final measurement uncertainties that depend upon the material and technique applied

• Compare and discuss the different approaches in uncertainty estimation • Consistency of measurements carried out by nuclear laboratories and by

operators with the GUM approach (ITV2010) • Focus on exchange between reference measurement institutes, safeguards

laboratories, nuclear and environmental material analysts and, in particular, operators

• Final report to be published in the ESARDA Bulletin, June 2012


CETAMA – IRMM from 50 years….

CETAMA GT 03 « analyse du plutonium »• MP2, Pu isotopic

reference

materials

Interlaboratory comparisons• EQRAIN, REIMEP/NUSIMEP

CETAMA GT 12 « spectrométrie de masse »

IAEA Consultants’ Group on nuclear RMs for safeguards verification measurements by Destructive Analysis (DA)

ESARDA Working Group for Techniques and Standards for Destructive Analysis (WGDA)

• First CETAMA-IAEA EQRAIN on impurities in uranium• Revision of International Target Values 2010• Dedicated workshops (U minors, impurity in U, LA-ICP-MS, ITVs,….)


CETAMA GT 03 « analyse du plutonium »• MP4, new Pu isotopic

reference

materials

Interlaboratory comparisons• EQRAIN, REIMEP/NUSIMEP

CETAMA GT 12 « spectrométrie de masse »• Advancement

in mass spectrometry

techniques

CETAMA GTXX « incertitude »• Estimation of measurement

uncertainties

according

to GUM

CETAMA – IRMM ….to 100 years


IAEA Consultants’ Group on nuclear RMs for safeguards verification measurements by Destructive Analysis (DA)

• Future needs

for reference

materials

and interlaboratory

comparisons

ESARDA Working Group for Techniques and Standards for Destructive Analysis (WGDA)

• Revision of International Target Values 2020, 2030, 2040, 2050, 2060• Technical convergence nuclear safeguards, forensics, security

ESARDA academic course on Nuclear Safeguards and Non-Proliferation

• ESARDA course in France in 2012 ??

CETAMA – IRMM ….to 100 years


Acknowledgement

CETAMA GT: D Roudil, C Rigaux, JM Adnet and all membersESARDA WG DA: A Hanssens, G Granier, H Isnard and all membersIRMM: A Verbruggen, R Jakopič and all colleagues


CETAMA – 50 years

joint research centre (jrc) - cea/cea

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