Update of Gd-LS R&D at IHEP

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Update of Gd-LS R&D at IHEP Ding Yayun, Zhang Zhiyong, Cao Jun Institute of High Energy Physics, Chinese Academy of Sciences

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Update of Gd-LS R&D at IHEP. Ding Yayun, Zhang Zhiyong, Cao Jun. Institute of High Energy Physics, Chinese Academy of Sciences. Quality Requirements for Gd-LS. – long attenuation length – good light yield – chemically compatible with acrylic – stable for several years. - PowerPoint PPT Presentation

Transcript of Update of Gd-LS R&D at IHEP

Page 1: Update of Gd-LS R&D at IHEP

Update of Gd-LS R&D at IHEP

Ding Yayun, Zhang Zhiyong, Cao Jun

Institute of High Energy Physics,

Chinese Academy of Sciences

Page 2: Update of Gd-LS R&D at IHEP

Quality Requirements for Gd-LS

– long attenuation length– good light yield– chemically compatible with acrylic– stable for several years

Two main concerns in the preparation of Gd-LS

– to find out the suitable solvents

– to find out the suitable Gd complexes with organic ligands

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Choice of Solvents

pseudocumene, PC and mesitylene

Drawbacks: low flash point

aggressive to acrylic

Linear alkylbenzene, LAB

high light yield, high flash point, low toxicity, cheap

long attenuation length

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Linear alkylbenzene , LAB, C10~C13

Produced by JinLing Petrochemical Limited Corp.,

SINOPEC Crop. P.R.C

Meet national standards GB/T 5177.5-2002

Elemental analysis shows:

C: 87.3% H: 11.5% (deviation: 1~3%)

The most possible average molecular formula is

C6H5-C12H25

Further study about the composition of LAB is ongoing.

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Requirements for the Selected Gd Complexes

– stable enough against hydroylsis

– relatively high solubility in aromatic solvent

– low absorption around 430 nm

– Organophosphorous compounds

– -Diketones

– Carboxylic acids

Three kinds of organic ligands have been used

Choice of Gd Complexes

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Organophosphorus Ligands

Triethylphosphate (TEP)

Triisoamylphosphine Oxide (TiAPO)

Dibutylbutylphosponate (DBBP)

Tri-n-octylphosphine oxide (TOPO)

Di(2-ethylhexyl) phosphate (D2EHP)

-Highly soluble in aromatic solvents

-Moderate attenuation length

P OR

R

R

P

O

RR

R

P

RR

R

Ln3+

O

Gd3+

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-Diketone

Acetylacetone (Acac) Chooz-II

Low solubility in the scintillator solvent

HC OC

R

R' CO

CH

O

CR R'

C

O

CH

OC R

R'

CO

Ln3+

_

_

_

Gd3+

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Carboxylic acids

2-Methylvaleric acid (2-MVA) 6C

BNL, IPCE-RAS, Chooz-II

2-ethylhexanoic acid (EHA) 8C

Bicron, Palo Verdo

3, 5, 5-trimethylhexanoic acid (TMHA) 9C

MPIK

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Preparation of Gd-CBX

1. Direct synthesis (Bicron, Palo Verdo, Chooz-II)

1) HA + NH4OH → NH4A + H2O

2) 3NH4A + GdCl3 → GdA3 + 3NH4Cl

2. Liquid-liquid extraction (BNL, MPIK)

Organic phase

Water phase

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Gd carboxylate complexes synthesized

Gd complexes with 2-ethylhexanoic acid (EHA)

white powder

Gd complexes with 3, 5, 5-trimethylhexanoic acid (TMHA)

white powder

Composition of the complexes

Gd-L3

L = EHA, TMHAMeasured by Elemental Analysis,

Vario EI, Elementar Analysensysteme GmbH

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Gd(TMHA)3 can be directly dissolved in LAB

Gd(EHA)3 only can be dissolved in the mixtures of

trimethylbenzene and LAB( or trimethylbenzene and dodecane)

Four Gd-LS samples have been prepared

Gd (g/L) Ligand fluors solvents

1.5 TMHA PPO5g/L

bis-MSB 10mg/LLAB

2.0 TMHA PPO5g/L

bis-MSB 10mg/LLAB

1.5 EHA PPO5g/L

bis-MSB 10mg/LVmesitylene:VLAB=2:8

2.0 EHA PPO5g/L

bis-MSB 10mg/LVmesitylene:VLAB=2:8

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Characteristics of Gd-LS Based on Gd-EHA, TMHA

Pgeneral TU-1901 UV-Vis spectrophotometer

10 cm Quartz Sample Cuvettes

1 、 Absorption Measurements

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A is the absorption at 430 nm

Absorption Spectrum measured by TU-1901

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2 、 Attenuation Length Measurements by Vertical LED System

Vertical LED System needs larger volume of sample

Vertical LED System: 1L

UV-Vis spectrophotometer: 40mL

Vertical LED System can obtain more

accurate attenuation Length data than

ordinary UV-Vis spectrophotometer.

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sample name

Absorption Measurement Vertical LED System

Abs

@ 430nm

Calculated Attenuation Length/m

Attenuation Length/m

LAB

(unpurified )

0.0053

±0.00028.2±0.3 8.7±0.6

LAB

(filtered)

0.0054

±0.00038.0 ±0.4 9.0±1.0

LAB+PPO

+bis-MSB

(filtered)

0.0062

±0.00017.0±0.1 7.1±0.4

Comparison of two methods for measuring Attenuation Length of the same Liquid samples

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3 、 Stability Test: 2g/L Gd-LS as a Function of Time

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4 、 Light Yield Measurements

Gd (g/L)

Ligand fluors solvents Relative Light Yield

- - PPO5g/L, bis-MSB 10mg/L Vmesitylene:VDodecane=2:8 0.459

- - PPO5g/L, bis-MSB 10mg/L LAB 0.542

1.5 EHA PPO5g/L, bis-MSB 10mg/L Vmesitylene:VLAB=2:8 0.538

2.0 EHA PPO5g/L, bis-MSB 10mg/L Vmesitylene:VLAB=2:8 0.528

1.5 TMHA PPO5g/L, bis-MSB 10mg/L LAB 0.492

2.0 TMHA PPO5g/L, bis-MSB 10mg/L LAB 0.478

relative light yield data = liquid scintillator / anthracene

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5 、 Emission Spectrum measurement

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Ongoing and Future R&D at IHEP

Continue our long-term stability tests for periods more than 1 year

Study the chemical compatibility of these Gd-LS with the materials that will be used to construct the detector vessel

Develop methods to remove radioactive impurities (10-10g/g)

Mass producition

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Thank You!Thank You!