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PS resins for the characterization of nuclear wastes: application to 126 Sn and 63 Ni Eduard Pelay, Ariadna Ferradal, Ignasi Villarroya, Héctor Bagán, Alex Tarancón, José F. García

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Page 1: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and

63Ni

Eduard Pelay, Ariadna Ferradal, Ignasi Villarroya, Héctor Bagán, Alex Tarancón, José F. García

Page 2: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Introduction

High number of nuclear facilities to be decommissioned

Necessity of new methods

126Sn: fission product importance in long term storage 63Ni: activation product high importance in decommissioning

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Introduction

• LS common technique for measurement of β emitters

• Problems of selectivity

chemical separations

• γ emitters easy to determine

• β and α some challenges

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

IntroductionPSm

alternative to LS for the measurement of high and medium energy radionuclides

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O

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Polymeric support

PS resins

unifies separation and measurement in a single step

immobilize selective extractants

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Objective

The objective of this study is to develop new PS resin follow new preparation procedures for the analysis of nuclear wastes

Page 6: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionExtractant

TBP in n-dodecane

Dissolves PSm

C-PS

126Sn

Tropolone

Stability problems

O

OH

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionImpregnation

TBP

Agitate 24 hFiltrate Rinse with H2O

n-dodecane

PSm

Page 8: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionProportion

0-100% TBP

Best PS resin proportion80% TBP0

20

40

60

80

100

100% 80% 60% 40% 20% 10% C- PSm

Sn re

tent

ion

(%) 0

20

40

60

80

100

20 40 60 80

Sn e

lute

d (%

)Total volume passed (mL)

100%

80%

60%

40%

20%

10%

C-PSm

Page 9: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionBatch medium determination

Optimum mediumHCl 2 M

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

0 1 2 3 4 5 6 7 8 9

Ret

entio

n(%

)

[HCl] (M)

Sn

Cs

Sb

Page 10: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionCalibration

Isotope Mean Energy (keV)

Detectionefficiency

(%)63Ni 17.43 15.514C 49.16 54.899Tc 94.60 81.736Cl 316.00 98.5

Isotope Mean Energy (keV)

Detectionefficiency

(%)126Sn 118.7 83.7

121mSn 120.7

y = -34.578x + 4.7249R² = 0.9986

0

1

2

3

4

5

0 0.02 0.04 0.06 0.08

ln(E

ff)

1/Emean (keV-1)

Ni-63

C-14

Tc-99

Cl-36

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionQuantification

Replicate Count rate(cpm)

Activity(dpm/g)

Quantification Error(%)

R1 420.00 5004 1.3R2 420.09 4943 2.5R3 412.46 4851 4.3

Mean 4933 ± 77

Quantitative retention

Isotopes Estimated Activity(dpm/g)

126Sn 79121mSn 4988241Am 56

Total activity 5067

Laboratoire Nationale Henry Becquerel

Page 12: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionPreparation strategy

Immobilization

63Ni

Imprinted

Covalent bound

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionImmobilization

DMG (2-1H-imidazol-2-il)piridina

With/without 1-octanol

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionResins properties

Best column:DMG

Resin Detection efficiency(%)Solution Evaporated

DMG + 1-octanol 11.0±1.1 29.4±1.5DMG 14.6±1.3 17.9±0.4iPyr + 1-octanol 8.1±1.0 12.4±1.1iPyr 7.9±0.6 27.6±1.5

0

20

40

60

80

100

DMG + 1-octanol DMG iPyr + 1-octanol iPyr

Rete

ntio

n (%

)

NiFeCo

Medium:Ammonium citrate pH 8

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionColumn analysis

Resin Total Efficiency (%)

DMG + 1-octanol 0.15 ± 0.04 DMG 0.54 ± 0.07

Total Efficiency = Detection Efficiency x Retention yield

Lost of the extractant

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionImprinted

VbIDA

polymerization rinse

Synthesis in presence of template

Selectivity based on steric impediment

No break through volumeUse of generic extractants

N COOH

COOH

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Results and discussionRetention

Medium:Ammonium

citrate pH 7-11

ResinDetection

efficiency(%) SQP(E)

Solution Evaporated Solution EvaporatedMIP 3.1±0.4 11.8±0.9 506.1 475.4

Optical quenching

0

20

40

60

80

100

7 9 10 11

Rete

ntio

n (%

)

pH

MIP Ni

Fe

Co

Preliminary results

High selectivity

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

N

N

N

Br

Results and discussionCovalent bound

Di-(2-picoyl)amine

HN

N

N

No break through volumeMore reproducible

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PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

Conclusions

A new PS resin for 126Sn determination has been developed

Different approaches for the preparation of a 63Ni PS resin were evaluated

MIP procedure shows a high selectivity

Page 20: PS resins for the characterization of nuclear wastes: application …lsc2017.nutech.dtu.dk/wp-content/uploads/7-Hector_UB_LSC... · 2017-05-12 · PS resins for the characterization

PS resins for the characterization of nuclear wastes: application to 126Sn and 63Ni

PS resins for the characterization of nuclear wastes: application to 126Sn and

63Ni

Eduard Pelay, Ariadna Ferradal, Ignasi Villarroya, Héctor Bagán, Alex Tarancón, José F. García

Acknowledgments

• Ministerio de Economia y Competitividad (MINECO) for financial support under CTM2014-02020

• Agència de Gestió d’Ajuts Uiversitaris i de Recerca (AGAUR) for financial support under 2014-SGR-1277.

• Dr. Philippe Cassette from LNHB (France) for supplying the 126Sn solution.