+ All Categories
Home > Documents > JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

Date post: 16-Apr-2022
Category:
Upload: others
View: 2 times
Download: 0 times
Share this document with a friend
20
JAEA-IAEA Workshop on Advanced Safeguards Technology for the Future Nuclear Fuel Cycle 13-16 November 2007, Ricotti, Tokai, Japan
Transcript
Page 1: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

JAEA-IAEA Workshop on Advanced Safeguards Technology for the Future Nuclear Fuel Cycle

13-16 November 2007, Ricotti, Tokai, Japan

Page 2: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

2

ContConteentsnts

Introduction of safeguards environmental sample analysis (ESA)

Objective of ESA in safeguardsTechnique of ESA

Bulk analysisParticle analysis (SIMS method)Particle analysis (FT-TIMS method)

Milestone Introduction of CLEAR facility

Page 3: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

3

IntroductionIntroduction

Suspicion for North Korea and Iraq in early 1990s93+2 Programme to strengthen the international safeguards system

Introduction of environmental sample analysis

Undeclared nuclear activitiesUndeclared nuclear materials

Page 4: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

4

Environmental sampleEnvironmental sample

Cotton cloth(10x10 cm2)

Cellulose(2.5cmφ)

Wipe wall and floor in a nuclear facility

High enrichment uranium in enrichment plantWeapon grade plutonium in R&D facility

Isotope ratio of U & Pu

For example, looking for

Page 5: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

5

LaboratoryLaboratory

CLEARClean room lab.Bulk analysisParticle analysisNon-radioactive sample

NUCEFRadiochemical lab.Bulk analysisRadioactive sample

Page 6: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

6

Environmental sample analysisEnvironmental sample analysis

Bulk Analysis

Particle Analysis

ICP-MS

SIMS

FT-TIMS

Cotton cloth(10x10 cm2)

Ashing ChemicalSeparation

Acidic Digestion

ISO Class 5 Clean roomAround 1 μm particles

DL for Pu : ~10 fg (10-15 g)

To remove matrix elements for accurate isotope ratio measurement

Page 7: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

7

Chemical separationChemical separation

Clean exhaust hood

15M HNO15M HNO33 && Dry up (3 times)Dry up (3 times)9.5M 9.5M HClHCl && Dry upDry up1M 1M HClHCl + 3M NH+ 3M NH22OHOH・・HClHClStanding for 60 min.Standing for 60 min.Dry up slowly Dry up slowly 9MHCl + 0.2M HNO9MHCl + 0.2M HNO33

22 9.5M 9.5M HClHCl

33 9M 9M HClHCl+ 0.1M HI+ 0.1M HI

Anion exchangeAnion exchangeMCI GEL, CA08P(75MCI GEL, CA08P(75~~150150μμmmφφ) 0.84ml) 0.84ml

44 0.5M 0.5M HClHCl

1212 Alkaline metal etcAlkaline metal etc 33 PuPu 44 UU

11 22 9M 9M HClHCl + 0.1M HNO+ 0.1M HNO33

Page 8: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

8

Isotope ratio measurementIsotope ratio measurement

100101102103104105106

Cou

nts

244242240238236234232MASS (A.M.U.)

Resolution (M/ΔM)= 300

0.32M HNO3 Solution1,800 cps / (pg/ml)

NU:5 ~ 800 pg/ml(ppt)

Ion detector:SEMScan mode:E-Scan

Double focus ICP-MS : ELEMENT1

Page 9: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

9

Bulk analysisBulk analysis (Radioactive(Radioactive sample)sample)

AshingAshing & Acid& AcidDigestionDigestion

22 0.70.7M HM HNONO33 + 90%CH+ 90%CH33OHOH

Anion exchangeAnion exchangeMCI GEL, CA08Y (25MCI GEL, CA08Y (25μμmmφφ), 50ml), 50ml

55 0.5M 0.5M HClHCl

1212 Alkaline metal etcAlkaline metal etc 33 UU 44 WasteWaste

11

22 9M 9M HClHCl + 0.1M HNO+ 0.1M HNO33

22 77M HM HNONO33

55 PuPu

33 77M HM HNONO33

RedoxRedox

TIMS

Page 10: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

10

Particle analysisParticle analysis

SIMS method (Routinely used)

試料台

2 μm O+

238U+

Particle recovery (Vacuum impactor)

Particles collected on planchet

SIMS

Page 11: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

11

MilestonesMilestones

2002 November Review at CLEARTwo IAEA experts visited JAEAAnalytical resultsFacility performance(CLEAR/NUCEF)QA/QC

2003 January Qualification to IAEA NWAL2003 February First analysis of domestic samples2004 January NWAL contract with IAEA2004 February First analysis of IAEA samples

Sample analysisBulk: 28 Swipes/y (Average 2005-2006)Particle: 33 Swipes/y (Average 2004-2006)

Page 12: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

12

DesolvationDesolvation modulemodule

http://www.elementalscientific.com/products/apex.asp

ApexHigh-efficiencyinlet system

Scott-type spray chamberSensitivity: 1.8 Mcps / ppb 238U

Sensitivity:13 Mcps / ppb 238U

Over 7 times improvement !!

Bulk analysis

Page 13: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

13

PickPick--up SIMS methodup SIMS method

Particle recovery (Vacuum impactor)

Particles pick up and transfer

Scanning electron microscopy(SEM)

Particles pick up

SIMS

Page 14: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

14

Results of pickResults of pick--up SIMSup SIMS

Pb

U

10 μm 10 μm

0.00015

0.00010

0.00005

0.00000

234 U

/238 U

isot

ope

ratio

10987654321Particle number

Natural uranium

0.00015

0.00010

0.00005

0.00000

234 U

/238 U

isot

ope

ratio

10987654321Particle number

Natural uranium

F.Esaka et al., Talanta 71 (2007) 1011.

Page 15: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

15

FTFT--TIMS methodTIMS method

Collect particles on filter

EtchingNeutron irradiation

Prepare irradiation sample

TIMS

Accurate methodA lot of time to measure

Page 16: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

16

X-ray tubeDetector

Swipe sampleUranium amount

Impurity measurement

Pb, Fe etc.

XRF for screeningXRF for screening

Page 17: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

17

X-ray spectrumEnergy (keV)

Inte

nsity

(x10

0 cp

s)

U-LαU-Lβ

U-Lγ

Semi-quantitative measurement

U, Pb, Fe etc.

Elemental distribution

5 x 7 mm

Uranium

Results of XRF measurementResults of XRF measurement

Page 18: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

18

CLEARCLEAR

Page 19: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

19

CLEARCLEAR –– Floor planFloor plan

Cleanness class is defined as maximum number of particles(> 0.5μm) in 1 ft3. No cleanness-controlled rooms, e.g. normal office rooms, sometimes contain the particle more than one million.

Page 20: JAEA-IAEA Workshop on Advanced Safeguards Technology for ...

20

Air flow and pressure controlAir flow and pressure control


Recommended