1、Designation: C1163 14Standard Practice forMounting Actinides for Alpha Spectrometry UsingNeodymium Fluoride1This standard is issued under the fixed designation C1163; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 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 covers the preparation of separated frac-tions of actinides for alpha spectrometry. It is applicable to anyo
3、f the actinides that can be dissolved in dilute hydrochloricacid. Examples of applicable samples would be the finalelution from an ion exchange separation or the final strip froma solvent extraction separation.21.2 The values stated in SI units are to be regarded asstandard. No other units of measur
4、ement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limit
5、ations prior to use. For a specifichazard statement, see Section 9.2. Referenced Documents2.1 ASTM Standards:3C859 Terminology Relating to Nuclear MaterialsC1284 Practice for Electrodeposition of the Actinides forAlpha SpectrometryD1193 Specification for Reagent WaterD3084 Practice for Alpha-Particl
6、e Spectrometry of Water3. Terminology3.1 For definitions of terms in this standard, refer toTerminology C859.4. Summary of Test Method4.1 Guidance is provided for the sample mounting ofseparated actinides using coprecipitation with neodymiumfluoride. The purified samples are prepared and mounted on
7、amembrane filter to produce a deposit that yields alpha spectraof sufficient quality for most analytical methodologies.Samples can be prepared more rapidly using coprecipitationthan by electrodeposition and have comparable resolution.5. Significance and Use5.1 The determination of actinides by alpha
8、 spectrometry isan essential function of many environmental and other pro-grams. Alpha spectrometry allows the identification and quan-tification of most alpha-emitting actinides. Although numerousseparation methods are used, the final sample preparationtechnique has historically been by electrodepo
9、sition (PracticeC1284). However, electrodeposition may have somedrawbacks, such as time required, incompatibility with priorchemistry, thick deposits, and low recoveries. These problemsmay be minimized by using the neodymium fluoride copre-cipitation method whose performance is well documented(1-6).
10、4To a lesser extent cerium fluoride has been used (7) butis not addressed in this practice.5.2 The sample mounting technique described in this prac-tice is rapid, adds an additional purification step, since onlythose elements that form insoluble fluorides are mounted, andthe sample and filter media
11、can be dissolved and remounted ifproblems occur. The recoveries are better and resolutionapproaches normal in electrodeposited samples. Recoveries aresufficiently high that for survey work, if quantitative recoveriesare not necessary, tracers can be omitted. Drawbacks to thistechnique include use of
12、 very hazardous hydrofluoric acid andthe possibility of a non-reproducible and ill-defined countinggeometry from filters that are not flat and may not be suitablefor long retention. Also, although the total turn around time forcoprecipitation may be less than for electrodeposition, copre-cipitation
13、requires more time and attention from the analyst.6. Interferences6.1 Calculation of a result from a sample that gives poorresolution should not be attempted since it probably implies anerror in performing the separation or mounting procedure.1This practice is under the jurisdiction of ASTM Committe
14、e C26 on the NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved June 1, 2014. Published July 2014. Originally approvedin 1992. Last previous edition approved in 2008 as C1163 08. DOI: 10.1520/C1163-14.2Hindman, F. D., “Actinide Separa
15、tions for Spectrometry Using NeodymiumFluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 12381241.3For 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 st
16、andards Document Summary page onthe ASTM website.4The boldface numbers in parentheses refer to a list of references at the end ofthis standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Apparatus7.1 Alpha SpectrometerA system
17、should be assembledthat is capable of 60 to 70 keV resolution on an actual sampleprepared by this practice, have a counting efficiency of greaterthan 20 %, and a background of less than 0.005 cpm over eachdesignated energy region. Resolution is defined as the full-width at half-maximum (FWHM) in keV
18、, or the distancebetween those points on either side of the alpha energy peakwhere the count is equal to one-half the maximum count.Additional information can be found in Practice D3084.7.2 Filter25-mm 0.1 m pore, polypropylene membranefilter or equivalent that will provide suitable alpha spectrom-e
19、try resoltuion.57.3 Vacuum FunnelPolysulfone twist-lock with stainlesssteel screen for filter mounting.57.4 Ultrasonic Bath.7.5 Plastic Centrifuge Tube, 50 mL.7.6 Stainless Steel Disk, 2.54 cm diameter.7.7 Infrared Heat Lamp.7.8 Tape, double-sided.8. Reagents8.1 Purity of ReagentsReagent-grade chemi
20、cals must beused in all procedures. Unless otherwise indicated, all reagentsshould conform to the specifications of the Committee onAnalytical Reagents of theAmerican Chemical Society, if suchspecifications are available.6Other grades may be used, if it isascertained that the reagent is of sufficien
21、tly high purity topermit its use without reducing the accuracy of the determina-tion. All reagents should be stored in polypropylene bottles.8.2 Purity of WaterUnless otherwise indicated, watermeans reagent water as defined in Specification D1193, TypeIII.8.3 Reagent BlanksReagent blanks should be a
22、nalyzed todetermine their contribution to the sample result.8.4 Neodymium Chloride Stock Solution (10 mg Nd/mL)Heat 25 mL of 12M hydrochloric acid and 1.17 g of neo-dymium oxide on a hotplate until the neodymium oxide is insolution. Cool the solution and dilute to 100 mL with water.8.5 Neodymium Chl
23、oride Carrier Solution (0.5 mg Nd/mL)Dilute 5 mL of the 10 mg Nd/mL neodymium chloridestock solution to 100 mL with water.8.6 Carbon SuspensionFume ten 47-mm cellulose filters7for about 10 min in 10 mL of 18M sulfuric acid. Cool thesuspension and dilute to 500 mL with water. The carbonsuspension is
24、used as a visual aid in identifying the presence ofthe precipitate.8.7 Substrate SolutionDilute 1 mL of the 10-mg Nd/mLneodymium chloride and 20 mL of 12M hydrochloric acid to400 mL with water. Add, with swirling, 10 mL of 29Mhydrofluoric acid and 8 mL of the carbon suspension. Dilutethe suspension
25、to 500 mL with water. Each day before use,place the substrate suspension in a sonic bath for 15 min.8.8 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (12M HCl).8.9 3M Hydrochloric AcidAdd 250 mL concentrated hy-drochloric acid to water and dilute to 1 L with water.8.10 Sulfuric Acid
26、(sp gr 1.84)Concentrated sulfuric acid(18M H2SO4).8.11 Hydrofluoric Acid (48 %)Concentrated hydrofluoricacid (29M HF). WarningSevere burns can result fromexposure of skin to concentrated hydrofluoric acid.8.12 Neodymium Oxide (Nd2O3).8.13 80 % Ethanol.8.14 20 % Titanium TrichlorideAvailable as a 20
27、% solu-tion of titanium trichloride from commercial suppliers.8.15 Sodium Sulfate SolutionDissolve 52 g of anhydroussodium sulfate in 500 mL of 18M sulfuric acid.8.16 Safranine-0 Solution, 0.1 %Dissolve 0.1 g ofsafranine-0 in 100 mL of water.9. Hazards9.1 WarningAdequate laboratory facilities, such
28、as fumehoods and controlled ventilation, along with safe techniquesmust be used in this procedure. Extreme care should beexercised in using hydrofluoric and other hot, concentratedacids. Use of rubber gloves is recommended.9.2 Hydrofluoric acid is a highly corrosive acid that canseverely burn skin,
29、eyes, and mucous membranes. Hydroflu-oric acid differs from other acids because the fluoride ionreadily penetrates the skin, causing destruction of deep tissuelayers. Unlike other acids that are rapidly neutralized, hydro-fluoric acid reactions with tissue may continue for days if leftuntreated. Fam
30、iliarization and compliance with the Safety DataSheet is essential.10. Sample Preparation10.1 Add 2 mL of sodium sulfate solution to the actinidefraction and evaporate to complete dryness in a glass beaker.Cool to room temperature and add 10 mL of 3M HCl. Coverthe beaker with a watch glass, bring to
31、 a boil, and keep at aboiling temperature for 5 min.5The sole source of supply for filter media specifically evaluated for alphaspectrometry coprecipitation (RF-100-25PP01) is Eichrom Technologies, LLC,Lisle, IL. The described vacuum funnel is available from Pall Life Sciences, AnnArbor, MI, catalog
32、 numbers 4203 or 4204 as needed. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.6Reagent Chemicals, American Chemica
33、l Society Specifications, AmericanChemical 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. Pharm
34、acopeial Convention, Inc. (USPC), Rockville,MD.7Ga-6 Metricel or equivalent has been found suitable for this purpose.C1163 14210.2 Transfer the solution to a capped 50-mL plastic centri-fuge tube using about 2 mL of 3M HCl as a rinse. For uranium,follow procedure described in 10.6 10.8.10.3 Add 100
35、Lof the 0.5 mg/mLNd carrier solution to thetube. Gently shake the capped tube to mix the solution.10.4 Add 5 mL of 48 % HF to the solution in the tube andmix well by gently swirling the tube. Let stand at least 5 min.10.5 Proceed with mounting procedure (Section 11).10.6 Add 1 drop of 0.1 % safranin
36、e-0 and 2 drops titaniumtrichloride to the uranium solution. Uranium reduction isindicated by a change from a purple or blue to an almostcolorless solution. If this color change does not occur orpersist, add another drop or two of titanium trichloride.10.7 Add 100 Lof the 0.5 mg/mLNd carrier solutio
37、n to theuranium solution. Gently swirl the tube to mix the solution.10.8 Add 5 mL of 48 % HF to the uranium solution and mixwell by gently swirling the tube. Let stand at least 5 min. Areappearance of color at this step may indicate incompleteuranium reduction and require the addition of more titani
38、umtrichloride and additional neodymium chloride carrier solution.10.9 Proceed with mounting procedure (Section 11).11. Mounting Procedure11.1 Mount a 25-mm membrane filter on a stainless steelsupport in a polysulfone twist-lock funnel.11.2 With vacuum applied, draw about 2 mL of 80 %ethanol through
39、the filter.11.3 As the filter becomes dry, add the following solutions,in order, to the center of the filter:11.3.1 Five mL of the substrate solution which has beenfreshly treated for 15 min in a sonic bath,11.3.2 The vigorously stirred sample from a capped tube,11.3.3 Five mL of 3M HCl is used to r
40、inse the samplecontainer,11.3.4 Five mL of water is used to rinse the samplecontainer, and11.3.5 Two mL of 80 % ethanol is used to rinse the filter.11.4 Dry the filter for 5 min under an infra-red heat lamp ata distance of 30 to 40 cm. Excess heating in drying will distortthe filter.11.5 Apply a 2.5
41、4 cm wide double-sided tape8to one side ofa clean, 2.54 cm diameter, stainless steel disk. Trim the tapeflush with the edge of the disk using a blade or knife. Centerthe dried filter on the taped side of the disk. Attach the filter tothe tape by gently pressing the edge of the filter in severalplace
42、s with the tip of a forceps or tweezers.11.6 Submit the sample for alpha spectrometry.12. Precision and Bias12.1 This practice addresses an intermediate step in anoverall separation and measurement scheme and does notproduce a measurement. Hence, a statement of precision andbias is not meaningful.13
43、. Keywords13.1 actinides; alpha particle; alpha spectrometry; ceriumfluoride; energy resolution; neodymium fluorideREFERENCES(1) Sill, C. W., “Precipitation of Actinides as Fluorides or Hydroxides forHigh-Resolution Alpha Spectrometry,” Nuclear and Chemical WasteManagement, Vol 7, 1987, pp. 201215.(
44、2) Hindman, F. D., “Actinide Separations for Spectrometry UsingNeodymium Fluoride Coprecipitation,” Analytical Chemistry, Vol 58,1986, pp. 12381241.(3) Rao, R. R., and Cooper, E. L., “Separation of Low Levels ofActinidesby Selective Oxidation / Reduction and Co-precipitation with Neo-dymium Fluoride
45、,” Journal of Radioanalytical and NuclearChemistry, Articles, Vol 197, No. 1, 1995, pp. 133148.(4) Kaye, J. H., Strebin, R. S., and Orr, R. D., “Rapid, QuantitativeAnalysis of Americium, Curium, and Plutonium Isotopes in HanfordSamples Using Extraction Chromatography and Precipitation Platin,”Journa
46、l of Radioanalytical and Nuclear Chemistry, Articles, Vol 194,No. 1, 1995, pp. 191196.(5) Nilsson, H., Rameback, H., and Skalberg, M., “An Improved Methodfor -Source Preparation Using Neodymium FluorideCoprecipitation,” Nuclear Instruments and Methods in Physics Re-search A, Vol 462, 2001, pp. 39740
47、4.(6) Lieberman, R., and Moghissi, A. A., “Coprecipitation Technique forAlpha Spectroscopic Determination of Uranium, Thorium, andPlutonium,” Health Physics, Vol 15, 1968, pp. 359362.(7) Maxwell, S. L., Culligan, B. K., and Noyes, G. W., “Rapid SeparationMethod for237Np and Pu Isotopes in Large Soil
48、 Samples,” AppliedRadiation and Isotopes, Vol 69, 2011, pp. 917923.8Scotch 665 has been found suitable for this purpose.C1163 143ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard ar
49、e expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeti
