ASTM C1414-2001(2014) Standard Practice for The Separation of Americium from Plutonium by Ion Exchange《用离子交换法从钚中分离镅的标准操作规程》.pdf

1、Designation: C1414 01 (Reapproved 2014)Standard Practice forThe Separation of Americium from Plutonium by IonExchange1This standard is issued under the fixed designation C1414; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye

2、ar of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice describes the use of an ion exchangetechnique to separate plutonium from solutions containing lowc

3、oncentrations of americium prior to measurement ofthe241Am by gamma counting.1.2 This practice covers the removal of plutonium, but notall the other radioactive isotopes that may interfere in thedetermination of241Am.1.3 This practice can be used when241Am is to be deter-mined in samples in which th

4、e plutonium is in the form ofmetal, oxide, or other solid provided that the solid is appropri-ately sampled and dissolved (See Test Methods C758, C759,and C1168).1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the u

5、ser of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C758 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNucl

6、ear-Grade Plutonium MetalC759 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC1168 Practice for Preparation and Dissolution of PlutoniumMaterials for AnalysisC1268 Test Method for Quantitative Determinatio

7、n of Am-ericium 241 in Plutonium by Gamma-Ray SpectrometryD1193 Specification for Reagent Water3. Summary of Practice3.1 Plutonium is adsorbed from a nitric acid (HNO3) solu-tion (8 M) onto an anion exchange resin. Under theseconditions, a negligible amount of americium is adsorbed ontothe resin and

8、 may be determined by gamma counting of theeluate using Test Method C1268.4. Significance and Use4.1 This practice is applicable when small amountsof241Am are present in plutonium samples (see Test MethodsC758 and C759). An example is the determination of241Am ina238Pu sample. The high specific acti

9、vity of238Pu presents asafety hazard that precludes its presence in a counting facility.Therefore, it is necessary to remove the238Pu prior to thedetermination of241Am.4.2 When a plutonium solution contains fission or activationproducts, this practice does not separate all radionuclides thatinterfer

10、e in the determination of241Am, such as the rare earths.5. Interferences5.1 The presence of other gamma-ray emitting radionu-clides similar in energy to241Am or that interfere with gammacounting make the determination of241Am less accurate. Most+4 valence actinides are adsorbed on the resin. The dis

11、tributioncoefficient for Am on this resin in nitric acid is less than 1,indicating insignificant adsorption. Therefore, this practice willseparate many elements that might interfere with gammacounting of241Am.5.1.1 The elements thorium, neptunium (IV), gold,platinum, iridium, and palladium are not q

12、uantitatively sepa-rated from plutonium by this procedure.6. Apparatus6.1 Anion exchange resin column (100-200 mesh), contain-ing quaternary ammonium functional groups (basic resin-chloride ionic form).36.2 Bottles, polyethylene, 30 mL.6.3 Sample beaker, 30 mL, borosilicate glass.1This practice is u

13、nder the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1999. Last previous edition approved in 2007 as C1414 01 (2007).DOI: 10.152

14、0/C1414-01R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Prefilled columns packed with AG 1-X8, availab

15、le from Bio-Rad, Richmond,CA, have been found to be acceptable.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.4 Hot plate.7. Reagents7.1 Purity of ReagentsReagent grade chemicals should beused in all tests. Unless otherwise indicat

16、ed, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.4Other grades may be used,provided that the reagent is first demonstrated to be ofsufficiently high purity to permit its u

17、se without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled or deionizedwater (Specification D1193).7.3 Nitric acid (HNO3), concentrated (sp gr 1.42).7.4 Hydrochloric acid (HCl), concentrated (sp gr 1.1

18、9).7.5 Nitric acid, 0.1 M. Add 6 mL of concentrated HNO3(spgr 1.42) to 950 mL of water and dilute to 1 L.7.6 Nitric acid 8 M. Add 500 mL of concentrated HNO3(spgr 1.42) to 400 mL of water and dilute to 1 L.7.7 Hydrofluoric acid (HF), concentrated (sp. gr. 1.18).7.8 Strip solution, 0.1 M HCl/0.01 M H

19、F. Add 8.3 mL ofconcentrated HCl (sp gr. 1.19) and 0.4 mL (6 to 7 drops) ofconcentrated HF to 950 mL of water and dilute to 1 L.8. Procedure8.1 Prepare a plutonium solution by following the procedurein Practice C1168 or by using another suitable dissolutiontechnique. Transfer an aliquot of the pluto

20、nium solution to a 30mL beaker. The amount of plutonium must be less than theadsorption capacity of the ion exchange resin. A maximum of50 mg of plutonium is suggested for the prefilled columns.8.2 Evaporate the sample to dryness on a hot plate. Add 3-4mL of 8 M HNO3and take to dryness again. Cool t

21、he sampleto room temperature and repeat the dissolution and evaporationonce more before proceeding to 8.3.8.3 Condition a prefilled anion exchange column by adding3-5 mL of 8 M HNO3and allow to drain. Discard the eluant.8.4 Position a clean 1 oz polyethylene bottle beneath thecolumn to collect the e

22、ffluent. Dissolve the plutonium samplein beaker containing 3-4 mL of 8 M HNO3. Transfer contentsof the beaker to the preconditioned ion exchange column.8.5 Allow solution to drain into the bottle. Rinse beakerwith 3-4 mL of 8 M HNO3. Transfer the rinse from the beakerto a column and allow the soluti

23、on to drain into a bottle. Repeatthis process twice more, allowing column to drain betweenadditions before proceeding to 8.6.8.6 Add 10 mL of 8 M HNO3directly to the column for thefinal rinse and allow to drain. Remove the bottle and addsufficient 8 M HNO3to make a total volume equal to 25 6 2mL.8.7

24、 Survey the bottle for external contamination.8.7.1 If bottle exterior is found to be contaminated, clean toacceptable levels of activity and transfer to a counting facility.8.7.2 If no contamination is found, transfer the bottle to acounting facility and determine the activity of gamma countingacco

25、rding to Test Method C1268.8.8 Strip the plutonium from the column with three 5 mLaliquots of 0.1 M HNO3or 1.0 M HCl/0.01 M HF.5Discard thecolumn and place the plutonium in the appropriate wastestream, or keep for further analysis.9. Keywords9.1 americium; gamma counting; ion exchange; plutoniumsolu

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29、mmittee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveadd

30、ress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).4Reagent Chemicals, American Chemical Society Specifications, A

31、mericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.50.1 M HCl/0.01 M HF is used when a more complete removal of plutoniumfrom the ion exchange resin is desired.C1414 01 (2014)2