Radiochemistry in Nuclear Power Reactors (1996) / Chapter Skim
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E. SELECTED RADIOCHEMICAL PROCEEDURES
E. SELECTED RADIOCHEMICAL PROCEEDURES
Pages 251-277
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From page 251... ...
Appendix E SELECTED RADIOCHEMICAL PROCEDURES E ~Determination of Radioactive Iodine in Water E.2 Determination of Strontium-89/90 E.3 Determination of Tron-55 E.4 Determination of Nickel-63 E-IL Page No.
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In a 250 mid separatory funnel containing 100 mL water sample (Note 3) , add 2 mL of I- carrier solution, 2 mL of NaOH, and 4 mL of NaOC1.
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Add 20 mL water containing a 1 mL cone. HNO3 and shake for 2 minutes.
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Metcalf, "Radiochemical Studies of the Fission Products" Book 3, p. 1625, National Nuclear Energy Series.
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The following three procedures are described: Strontium separation (2) Yttrium separation (3)
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HNO3 and boil down to ~10 mL. Transfer solution to a 40 mL cone with H2O.
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k. Add 20 mL H2O to dissolve Sr(NO3~2 and add 6 drops of Fe scavenger carrier.
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cl. Add 10 drops of 0.IM AgNO3 and ~ mL cone.
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i. Add 5 mL cone.
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Pipet 25.0 mE Sr carrier and appropriate amount of Sr-90 stanciard into a 40 mL centrifuge cone.
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1. Place the flask on a magnetic stirring plate and stir solution gently.
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Acid ~8 mL cone.
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Add 2 mL sat. H3BO3 and 3 mL cone.
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Pipet desired volumes of slurry to a tare filter paper #542 and wash with 5 mL me tiny} alcohol. (A minimum of 10 samples with varying amounts of slurry should be orenarecl.)
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c.y.f. = chemicaly~eld factor, % yield eff = counting efficiency (see Figure E-1 )
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20 mg (9.0 mg/cm2) SAMPLES AS A FUNCTION OF AVERAGE BETA ENERGY 0.8 AVERAGE ENERGY, E 1 .C Figure E-1 Counting Efficiency Curves of Beta Activities Using WIDEBETA II E-16
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Iron isotopes Fe-55 and Fe-59 are separated from fission and corrosion products by ion exchange and organic extraction. The organic phase is then transferred into a counting vial containing toluene base scintillator cocktail.
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hold back carrier in a I-L beaker containing 500 mL water sample. (Note: If the sample is a solution from solid, or filter paper dissolution, use 20 mL sample solution and add all carrier as specified above.
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CAREFULLY watch for the yellow effluent and collect only THIS effluent into a 40 mL centrifuge tube.
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m. Transfer the organic layer with a pipes to a counting vial that contains 10 mL liquid scintillation cocktail solution.
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(Note: The energy discrimination settings are cletermineclby using pure Fe-55 and Fe-59 isotopes separately in the counting samples. The lower energy channel should include most of the Fe-55 counting but minimizing the interference from Fe-59 which is counted in the higher energy channel.)
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E.3.4 Reference (~)
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HCT - 6N concentrated NaOH- IN NH4OH- concentrated Anion resin - AG ~xI0 50-100 mesh chloride form Dimethylglyoxime - ~ % solution in Ethanol Liquid scintillation (POPOP solution) cocktail Toluene Chloroform Analytical filter paper pulp - Ash free Pyridine NH4SCN ~ % solution + Pyridine ~ % solution = rinse solution NH4SCN- 20% solution HAC- IN Alconex- 0.25% E-23
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To 500 mL of water sampled in a I-L beaker, add 500\ of Ni carrier, 4 ctrops each of Cs, Fe, Co and Mn hold-back carrier, and 3 mL cone.
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in separation procedure, slowly add cone. NH4OH until solution is just basic, using pH paper as indicator.
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Pipet 20 mL to a 40 mL centrifuge tube, add IN NaOH or IN HAc to adjust to pH ~7 using pH paper as indicator.
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d. Prepare a counting efficiency curve, i.e., efficiency vs.
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