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The Determination of 226Ra in Water Samples
Anil H. Thakkar & Michael Fern Eichrom Technologies, Inc. David McCurdy Duke Engineering & Services Basically this piece of work was carried for our potential client Quanterra, formerly known as IT Corp. A protocol was proposed to Quanterra based on their needs to carry out day to day analyses in their lab.
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Objectives To design a procedure for radium in water which would:
be a simple, short and quick procedure allow to measure Ra-226 and Ra-224 via alpha spectroscopy and Ra-228 via Ac-228 measurements eliminate the tedious steps of precipitation and metathesis An improved procedure was developed to separate Am,Pu and U in variety of water matrices.
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Current Procedure Used
Barium sulfate precipitation Conversion to BaCO3- tedious and time consuming
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Current Procedure Used
Sample + Ba carrier + Ba Conc.H2SO4_+ Heat BaSO4 Precipitate allowed to settle for several hours or overnight Precipitate collected and converted to BaCO3
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New Approach Water samples Cation exchange resin column
Eichrom Ln Resin column
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Preparation of Water Samples
0.5 L / 1.0 L water samples Acidified to pH 2 Add 133Ba as a tracer
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Eichrom Cation Exchange Column
Load solution: 0.5 L/ 1.0 L of sample Rinse with 50 mL of 0.1M HNO3 Strip Ra and Ba with 100 mL of 8M HNO3
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Preparation of Load Solution for Ln Resin Column
Evaporate eluent from cation exchange column to dryness Dissolve residue in 10 ml of 0.095M HNO3 acid Load on Eichrom Ln Resin column
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Ln Resin Column Separation
(1) Load: 10 mL of 0.095M HNO3, Collect (1) and (2) for Ba & 226Ra (2) Rinse: 15 mL of 0.095M HNO3 On Uteva spec, the actinides were loaded with a load solution of 3M HNO3/0.5 M Al(NO3)3 solution, Pu was reduce by Iron. Am/Pu pass thru, Uteva, therefore the load solution and rinse are collected, Uranium is stripped by 0.01 M HCl . (3) Strip: 10 mL of 0.35M HNO3 collect (3) for 228Ac
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226Ra Via Alpha Spectrometry
Evaporate 226Ra/133Ba fraction to 10 mL volume Add 0.1 ml of 0.75 mg/ml barium carrier Add 3 mL of 40% sodium sulfate, 4 drops of 1:1 acetic acid. Swirl Add 0.2 mL of seeding suspension. Mix Place tubes in cold water bath for 30 minutes Filter on 0.1 micron filters, count via alpha spectrometry
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eichrom 133Ba Via Gamma Counter
Count 133Ba tracer yield via gamma spectrometry
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228Ac Via Gas-Flow Proportional Counter
Add 50 micrograms of cerium carrier Add 1.0 mL of HF Filter on 0.1 micron filters Measure for beta radiation
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226Ra % Recoveries-0.5L DI Water
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226Ra Alpha Spectrum
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133Ba Gamma Spectrum
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226Ra, 224Ra, and Daughters 224Ra 226 Ra 220Rn 218Po 222Rn
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226Ra % Recoveries in Tap water
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226Ra in EPA Sample Sept.18, 1998
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226Ra in NJ Sample
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226Ra in Georgia Inst. Of Tech. Sample# S8933
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226Ra in Georgia Inst. Of Tech. Sample# WS 14776
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Ca and Mg Interference 50, 100, 200, 400 and 500 ppm of Ca and Mg solutions were tested 500 mL and 100 mL volumes tested
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Ca and Mg Interference in 500 mL Samples
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Ca Interference in 100 mL of Sample
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Detection Limits
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Summary <1.0 pCi/L detection limits achievable
A good replacement for BaSO4 precipitation Eliminates inconsistent metathesis steps Reduces usage of chemicals/reagents Provides consistency and saves time High amounts of Ca and Mg interferences handled well with 100 mL samples Acceptable 226Ra recoveries
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Acknowledgements Special thanks to Dr. B. Parsa, New Jersey department of health, NJ Dr. B. Kahn, Georgia Institute of Technology, GA
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