1、Designation: C 1163 08Standard Practice forMounting Actinides for Alpha Spectrometry UsingNeodymium Fluoride1This standard is issued under the fixed designation C 1163; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 as an alternate toelect
3、rodeposition. It is applicable to any of the actinides thatcan be dissolved in dilute hydrochloric acid. Examples ofapplicable samples would be the final elution from an ionexchange separation or the final strip from a solvent extractionseparation.21.2 The values stated in SI units are to be regarde
4、d asstandard. No other units of measurement 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
5、the applica-bility of regulatory limitations prior to use. For a specifichazard statement, see Section 9.2. Referenced Documents2.1 ASTM Standards:3C 859 Terminology Relating to Nuclear Materials4D 1193 Specification for Reagent WaterD 3084 Practice for Alpha-Particle Spectrometry of Water3. Termino
6、logy3.1 For definitions of terms in this standard, refer toTerminology C 859.4. 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 amembrane filter to produce a de
7、posit that yields alpha spectraequal to electrodeposited samples. Samples can be preparedmore rapidly than by electrodeposition and have comparableresolution.5. Significance and Use5.1 The determination of actinides by alpha spectrometry isan essential function of many environmental programs. Alphas
8、pectrometry allows the identification and quantification ofmost alpha-emitting actinides. Although numerous separationmethods are used, the final sample preparation technique hashistorically been by electrodeposition. However, electrodepo-sition may have some drawbacks, such as time required,incompa
9、tibility with prior chemistry, thick deposits, and lowrecoveries. These problems may be minimized using theneodymium fluoride method.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 ar
10、e mounted, andthe sample and filter media can be dissolved and remounted ifproblems occur. The recoveries are better and resolutionapproaches normal electrodeposited samples. Recoveries aresufficiently high that for survey work, if quantitative recoveriesare not necessary, tracers can be omitted. Dr
11、awbacks to thistechnique include use of very hazardous hydrofluoric acid andthe possibility of a non-reproducible and ill-defined countinggeometry from filters that are not flat. Also, although the totalturn around time for coprecipitation may be less than forelectrodeposition, coprecipitation requi
12、res more time and at-tention 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 CommitteeC26
13、 on the NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved July 15, 2008. Published August 2008. Originallyapproved in 1992. Last previous edition approved in 2003 as C 1163 03.2Hindman, F. D., “Actinide Separations for Alpha Spectrom
14、etry Using Neody-mium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 12361241.3For 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 standards Document
15、 Summary page onthe ASTM website.4Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Apparatus7.1 Alpha SpectrometerA system should be assembledthat is capable of 60 to 70 keV resolution on an actual sampleprepared by this
16、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, or the distancebetween those points on either side of the alpha energy peakwhere the count is eq
17、ual to one-half the maximum count.Additional information can be found in Practice D 3084.7.2 Filter25-mm 0.1 m pore, polypropylene membranefilter or equivalent.57.3 Vacuum FunnelPolysulfone twist-lock with stainlesssteel screen for filter mounting.57.4 Ultrasonic Bath.8. Reagents8.1 Purity of Reagen
18、tsReagent-grade chemicals 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 re
19、agent is of sufficiently 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 D 1193, TypeIII.8.3 Reagent BlanksReag
20、ent blanks should be analyzed todetermine their contribution to the sample result.8.4 Neodymium Chloride Stock Solution (10 mg Nd/mL)Heat 25 mL of 12N hydrochloric acid and 1.17 g of neody-mium oxide on a hotplate until the neodymium oxide is insolution. Cool the solution and dilute to 100 mL with w
21、ater.8.5 Neodymium Chloride 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. Th
22、e carbonsuspension is 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.
23、 Dilutethe suspension 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 3N Hydrochloric AcidAdd 250 mL concentrated hy-drochloric acid to water and dilute to 1 L with wat
24、er.8.10 Sulfuric Acid (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 Trichlo
25、rideAvailable as a 20 % 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 labora
26、tory facilities, such 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 c
27、anseverely burn skin, eyes, and mucous membranes. Hydrofluo-ric acid is similar to other acids in that the initial extent of aburn depends on the concentration, the temperature, and theduration of contact with the acid. Hydrofluoric acid differsfrom other acids because the fluoride ion readily penet
28、rates theskin, causing destruction of deep tissue layers. Unlike otheracids that are rapidly neutralized, hydrofluoric acid reactionswith tissue may continue for days if left untreated. Due to theserious consequences of hydrofluoric acid burns, prevention ofexposure or injury of personnel is the pri
29、mary goal. Utilizationof appropriate laboratory controls (hoods) and wearing ad-equate personnel protective equipment to protect from skin andeye contact is essential.10. Sample Preparation10.1 Add 2 mL of sodium sulfate solution to the actinidefraction and evaporate to complete dryness in a glass b
30、eaker.Cool to room temperature and add 10 mL of 3 N HCl. Coverthe beaker with a watch glass, bring to a boil, and keep at aboiling temperature for 5 min.10.2 Transfer the solution to a capped 50-mL plastic centri-fuge tube using about 2 mL of 3N HCl as a rinse. For uranium,follow procedure described
31、 in 10.6-10.8.10.3 Add 100 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 A
32、dd 1 drop of 0.1 % safranine-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
33、0.5 mg/mLNd carrier solution to theuranium solution. Gently swirl the tube to mix the solution.5Available from Pall Life Sciences, Ann Arbor, MI, catalog number M5PU025.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the test
34、ing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.7Ga-6 Metricel or equivalent has been found suit
35、able for this purpose.C116308210.8 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 titaniumtrichloride and additional neodymium
36、 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 the filter.11.3 As the filter becomes
37、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 3N HCI is used to rinse the samplecontainer,11.3.4 Five m
38、L 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 12 to 16 in. Excess heating in drying will distortthe filter.11.5 Apply a 2.54 cm wide double-coated cellophane typ
39、etape8to one side of a clean, 2.54 cm diameter, stainless steeldisk. Trim the tape flush with the edge of the disk using a bladeor knife. Center the dried filter on the taped side of the disk.Attach the filter to the tape by gently pressing the edge of thefilter in several places with the tip of a f
40、orceps 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.ASTM International take
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42、ponsibility.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 address
43、ed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the
44、 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 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).8Scotch 665 has been found suitable for this purpose.C1163083
