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The Rapid Determination of Strontium-89 and Strontium-90 in Environmental Samples

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The Rapid Determination of Strontium-89 and Strontium-90 in Environmental Samples The Rapid Determination of Strontium-89 and Strontium-90 in Environmental Samples Terence O’Brien*, Lawrence Jassin, E. Philip Horwitz and Daniel McAlister Eichrom Technologies and PGRF Presented at www.alarasolutions.comthe MARC IX: Conference Kailua-Kona, HI March 29, 2012 www.eichrom.com Monday, December 6th, 2011: Japan Today Some 45 tons of highly radioactive water The utility is testing seawater samples leaked Sunday from desalination taken off the coast near the plant to see equipment used to decontaminate the if it is contaminated with strontium. radioactive water in Tokyo Electric Power It will know the results in about Co.'s Fukushima No. 1 nuclear plant and two to three weeks, Tepco said. it is unclear if any made it to the sea, a Tepco official said Monday… www.eichrom.com Strontium-89 & Strontium-90 www.eichrom.com Strontium-89 & Strontium-90 Strontium-89 Strontium-90 T1/2 = 50.53 days T1/2 = 28.90 years Mean Beta energy = 584.6 keV Mean Beta Energy = 195.8 keV Mean beta-dose = 0.5846 MeV/Bq-s Mean beta-dose = 0.196 Daughter Yttrium-89 Stable MeV/Bq-s Daughter Yttrium-90 T1/2 = 64.0 hours Mean Beta Energy = 933.6 keV Mean beta-dose = 0.9336 MeV/Bq-s Daughter Zirconium-90 Stable www.eichrom.com The Issues Some methods for the determination of radioactive strontium take one of the following approaches. 1. Rapid Radiochemical Method for Total Radiostrontium (Sr-90) in Water for Environmental Restoration Following Homeland Security Events: 2.2.1 This test assumes that it is reasonable to assume the absence of 89Sr in the sample. 2. Eichrom SRW01 – Strontium 89, 90 in Water 7.9.3 “After yttrium ingrowth of approximately 1 week” www.eichrom.com The Issues 3. Rapid separation of actinides and radiostrontium in vegetation samples If 89/90Sr differentiation is needed, there are Čerenkov counting techniques for more rapid determination of 89Sr and 90Sr. 89Sr can be measured directly by Čerenkov counting, employing methodology that takes advantage of the high Čerenkov counting efficiency of 89Sr relative to 90Sr [11]. www.eichrom.com Assumptions 1. Strontium-89 and Strontium-90 could be present in a sample. 2. Strontium-90 and Yttrium-90 will likely be in equilibrium. 3. Rapid sample turnaround required. – 8 Hrs 4. Many samples to be analyzed. – Multi- Detector www.eichrom.com 1st Tool: Preconcentration 1. For Sr Resin – Sr k’ around 80-90. Therefor sample volumes above 50 mL should be avoided to minimize Sr break through. 2. Water sample evaporation is an option but the clock is ticking. 3. Cation Exchange 4. A fast calcium phosphate precipitation can concentrate both Sr and Y. www.eichrom.com 2nd Tool: Sr Resin www.eichrom.com Sr Resin www.eichrom.com 3rd Tool: DGA Resin TRU Resin DGA Resin, Normal DGA Resin, Branched 6 6 6 10 10 10106 106 Ca(II) Pu 5 5 5 Sr(II) 10 10 10105 105 Ba(II) Th Ra(II) 4 4 4 10 10 10 4 4 Y(III) 10 10 Pu U Pu 3 3 3 10 10 10103 k' for Be and Mg < 1 103 for all [HNO ] Ca Th k' 3 k' k' Am k' for Be and Mg < 1 2 2 22 2 10 10 1010 Y(III) 10 Am Th for all [HCl] Sr Sr(II) 1 1 Am 11 1 10 10 1010 10 Ba U Pu(IV) Ra Sr U 0 Th(IV) 0 00 0 Ca 10 10 1010 Sr(II) 10 U(VI) Ba Am(III) Ra -1 -1 -1-1 -1 10 10 1010 10 -2 -1 0 1 -2 -1 0 1 -2 -2 -1 -1 0 0 1 1 -2-2 -1 -1 0 0 1 1 -2 -1 0 1 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 10 1010 1010 1010 1010 10 10 10 10 [HNO ] [HCl] [HNO ] [HNO ] [HNO[HNO ] ] [HCl] 3 3 3 3 3 www.eichrom.com 4th Tool Vacuum Box www.eichrom.com Sample flow rates 1. Recommended: Load/Elution 1 mL / min Rinse rates of 3 mL / min 2. 2007 RRMC - Julie Gostic reports work with flow rates of 6-7 mL/min with good recoveries for Am-241 on TRU and DGA 3. 2009 Maxwell publishes the use of 2-4 mL/min for rapid / emergency sample analysis. www.eichrom.com Flow Sheet: Rapid Sr-89 & Sr-90 Preconcentration Aliquot & Acidify <pH 2 Add Sr & Y Carrier/Tracer and Matrix Spikes Add Calcium Nitrate, Barium Chloride, Ammonium Phosphate, Phenolphthalein Add Concentrated Ammonium Hydroxide To dark pink phenolphthalein end point Centrifuge 2000-3000 rpm 5-10 minutes Pour off supernate Dissolve Precipitate with 8M Nitric Acid and 0.5M Aluminum Nitrate Dispose of Liquid www.eichrom.com Strontium / Yttrium Separation and Retention Precondition 8M HNO3 Dissolved Sample C-Tube Rinse Reservoir 8M HNO3•0.5M Al(NO3)3 Sr Resin Reservoir DGA Resin Vacuum Box Vacuum Box5 mL 3M HNO3 + 0.05M Oxalic Acid 5 mL 8M HNO3 Elution… 0.05M HNO3 www.eichrom.com Strontium Elution 1000 100 10 [Sr] in ppm[Sr] in 1 0.05M HNO3 - 96 %R 0.1 0.01 0 1 2 3 4 5 6 7 8 Free Bed Volumes www.eichrom.com Yttrium on DGA… Reservoir What could be there beside Y ? How do we get the DGA Y off without Resin interferences? Vacuum Box www.eichrom.com Load/Rinse 8 M HNO3 with 0.5M Aluminum Nitrate Rinse with 0.1M HNO3 Distribution coefficients (Kd) of 60 elements on TODGA resin in logarithmic scale as a function of HNO3 molaritywww.eichrom.com Secondary Rinse with 3M HCL Distribution coefficients (Kd) of 60 elements on TODGA resin in logarithmic scale as a function of HCl molarity www.eichrom.com Yttrium elution from DGA 1000.00 100.00 10.00 1M HCl - 27.1 %R 0.5M HCl - 86.2 %R [Y] in ppm 0.1M HCl - 90.8 %R 1.00 1M Acetic - 84.4 %R 0.5M Acetic - 88.1 %R 0.10 0.01 0 1 2 3 4 5 6 7 8 Bed Volumn www.eichrom.com Beta Detection LSC/Cherenkov GPC Low Background Counters www.eichrom.com Carrier Recoveries Matrix/Carrier Avg.Recovery RSD% De-ionized Water Strontium 84.9% 4% Yttrium -- -- Tap Water: Strontium 75.0% 7% Yttrium -- Waters; n=4 www.eichrom.com Yttrium and REEs Waters of Hydration Thermal Gravimetric Analysis The issue: C: Yttrium Oxalate has many waters of Hydration The solution: Conversion to Yttrium Oxide at 800 www.eichrom.com Sr-89 Sr-90 Certified Measured Difference Certified Measured Difference Sample Value Value ±% Value Value ±% Blank -0.35±0.37 0.30±023 De-ionized Water-A 2.8±1.2 +18 0.72±0.27 -40 2.39 1.20 De-ionized Water-B 2.4±1.0 +2 0.97±0.33 -19 ±0.05 ±0.02 De-ionized Water-C 2.0±.81 -16 1.21±0.38 +1 Tap Water-A 2.7±1.1 +13 1.12±0.38 -7 2.39 1.20 Tap Water-B 2.5±1.0 +5 1.24±0.39 3 ±0.05 ±0.02 Tap Water-C 3.1±1.3 +30 1.18±0.38 -2 Sample count time was 20 minutes and results are in Bq/L Estimated Time Line (10 samples) Step Minutes Elapsed Time (hrs) Sample Aliquot & Spiking 30 0:30 Sample Pre-Concentration 45+ 1:15 Sample Separation Sr & DGA 30 1:45 Sr Purification 30 2:15 Y Purification (Concurrent with 30 -- Sr Purification) Sample Mounting (Sr & Y) 45 3:00 Counting Time Sr-89 – 3.5 Bq/L MDA 20+ 3:20 Sr-90 – 3.0 Bq/L MDA Data Reduction 20 4:00 www.eichrom.com Future Work 1. Yttrium Yield Measurement Technique a) Oxalates and Hydroxides b) Gravimetric vs AA/ICP 2. Interference Rejection 3. Additional Matrix Preparation www.eichrom.com Acknowledgments Phil Horwitz, Dan McAlister, Larry Jassin at PRGF and Eichrom Tim Winters at GEL Labs Bob Shannon at Quality Radioanalytical Support Environmental Resource Associates Thank you for you attention and your questions. www.eichrom.com .
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