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Chromatographic Separation and Measurement of Charged-Particle Emitting Radionuclides. Timothy A. DeVol, Ph.D., C.H.P. Environmental Engineering and Science Clemson University 16 May 2000. Introduction to Dual Functionality Materials. Liquid Extractive Scintillators

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chromatographic separation and measurement of charged particle emitting radionuclides

Chromatographic Separation and Measurement of Charged-Particle Emitting Radionuclides

Timothy A. DeVol, Ph.D., C.H.P.

Environmental Engineering and Science

Clemson University

16 May 2000

introduction to dual functionality materials
Introduction to Dual Functionality Materials
  • Liquid Extractive Scintillators
    • Ludwick, Health Physics, 1961, 6, 63-65.
    • McDowell and McDowell, Liquid Scintillation Alpha Spectrometry, CRC Press, Boca Raton, 1994.
  • Scintillating Cation and Anion Ion Exchange Resin
    • Heimbuch, et al., Radioisotope Sample Measurement Techniques in Medicine and Biology, Proceedings of the International Atomic Energy Agency Symposium, Vienna, May 24-28, 1965.
  • Solid Extractive Scintillators for 90Sr and 99Tc
    • Egorov et al., Anal. Chem 71 (1999) 5420-5429
  • Solid Extractive Scintillators for 90Sr, 99TcandActinides
    • DeVol et al., Radioactivity&Radiochemistry Vol. 11 #1 (2000)
separation and detection schemes
Separation and Detection Schemes
  • Single scintillation crystal, e.g. CaF2:Eu, anthracene
  • Extractant coated onto inert scintillator
  • Mixture of extraction resin with granular scintillator
  • Extractant impregnated into a scintillating chromatographic resin (ScintEx)
solid extractive scintillators
Solid Extractive Scintillators
  • Sequential Extraction Chromatography and Flow-cell Detection Off-line quantification
  • Simultaneous Extraction Chromatography and Flow-cell Detection On-line quantification
materials and methods
Materials and Methods
  • Mixed-ResinMixture of:
    • 100 - 150 mm TEVA Resin or Sr Resin
    • 100 - 200 mm BC-400 Plastic Scintillation Beads (Bicron)or 63 - 90 mm GS-20 Scintillating Glass (Applied Scintillation Technology)
extractive scintillator resin
Extractive Scintillator Resin
  • ScintEx resin (Patent Pending)
    • Inert polystyrene chromatographic resin (Amberchrom CG-161c) impregnated with PPO and DM-POPOP using a modification of the Ross 1991 procedure
    • Scintillating chromatographic bead impregnated with extractant (Eichrom proprietary technology)
      • Extractant for Sr
      • ABEC-2000
      • Quaternary Amine, Aliquat-336 (TEVA)
      • CMPO extractant in TBP for actinides
off line evaluation procedures
Off-Line Evaluation Procedures
  • Resin dry packed into 9 mm x 50 mm opaque column
  • Conditioning, loading and wash performed with standard Eichrom procedures
  • Column placed in 7-mL HDPE vial WITHOUT introduction of LSC cocktail
  • Activity quantified with Hidex Triathler liquid scintillator counter
results and discussion
Results and Discussion
  • Mini-Column Experiments (Off-Line)
    • Compare pulse-height spectra (luminosity) and detection efficiency
  • Flow-Cell Experiments (On-Line)
    • Loading and elution profiles (loading and detection efficiency, and total recovery)
    • Regeneration capability
schematic of on line flow cell detection system

PMT

PMT

Schematic of On-Line Flow-Cell Detection System

Flow-cell

Manually controlled pump

Radiation Detector

Effluent

Loading

Solution

Eluant

Sample

Computer

LSC

extractive scintillator flow cell
Extractive Scintillator Flow-Cell

Extractive scintillator flow-cell

was constructed of with <0.5 g

of resin packed into 1.5 mm ID

x 140 mm polytetrafluoro-

ethylene tubing to yield an

approximate pore volume of

200-400 mL. The tubing is

coiled to an approximate

diameter of 2.54 cm and placed

between the photomultiplier

tubes of the radiation detector.

loading and elution of 99 tc teva bc 400 mixed resin flow cell 137 cs interference test
Loading and Elution of 99TcTEVA/BC-400 Mixed-Resin Flow-Cell137Cs Interference Test

99Tc; 5 mL; 24 Bq mL-1

137Cs; 1 mL; 7.2 kBq mL-1

multiple loading and elution of 89 sr on sr scintex o
Multiple Loading and Elution of 89Sr on Sr ScintEx O

Avg. Detection efficiency 60  4%

Avg. Loading efficiency 101 ± 1%

65.4%

58.8%

57.6%

59.6%

sequential elution of 241 am 239 pu and 233 u from tru scintex resin
Sequential Elution of 241Am, 239Pu and 233U from TRU ScintEx Resin

On-Line Counting

Off-Line Counting

conclusions
Conclusions
  • Extractive scintillator media can be realized a number of ways
  • Extractive scintillator media can be selective to analyte of interest
    • demonstrated with technetium-selective, strontium-selective and actinide-selective extractant
  • Loading, retention, and elution similar to non-scintillating resin
  • Quantification has been demonstrated on-line and off-line
  • Limited spectroscopy appears to be available with the actinide-selective ScintEx resin
  • Absolute detection efficiency ranges from ~40% for 90Sr to near 100% for actinide- selective ScintEx resin
acknowledgments
Acknowledgments
  • James Harvey, Eichrom IndustriesJonathan Duffey, formerly from Eichrom
  • From Clemson University:Robert Fjeld, Alena Paulenova (on leave from Comenius´ University, Slovak Republic), James Roane
  • John Leyba, WSRTC
  • NSF SBIR Phase I contract # NSF/SBIR-9760934
  • South Carolina University Education and Research Foundation TOA #KC86372-O.
  • DOE Environmental Management and Science Program, Project #70179