1、Designation: C1647 06C1647 13Standard Practice forRemoval of Uranium or Plutonium, or both, for ImpurityAssay in Uranium or Plutonium Materials1This standard is issued under the fixed designation C1647; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e case of revision, the year 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 covers instructions for using an extraction chromatography column method
3、 for the removal of plutonium oruranium, or both, from liquid or digested oxides or metals prior to impurity measurements. Quantification of impurities can bemade by techniques such as inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emissionspectrometry (ICP-
4、AES) or atomic absorption spectrometry (AAS.)1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibili
5、tyof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide PowderC757 Specification for Nuclear-G
6、rade Plutonium Dioxide Powder, SinterableC776 Specification for Sintered Uranium Dioxide PelletsC787 Specification for Uranium Hexafluoride for EnrichmentC788 Specification for Nuclear-Grade Uranyl Nitrate Solution or CrystalsC859 Terminology Relating to Nuclear MaterialsC996 Specification for Urani
7、um Hexafluoride Enriched to Less Than 5 % 235UC1168 Practice for Preparation and Dissolution of Plutonium Materials for AnalysisC1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled PlasmaMass SpectrometryC1347 Practice for Preparation and Dissol
8、ution of Uranium Materials for AnalysisC1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, andInductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) AnalysisC1517 Test Method for Determination of Metallic Impurities in Uranium
9、 Metal or Compounds by DC-Arc EmissionSpectroscopyD1193 Specification for Reagent Water3. Terminology3.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.4. Summary of Practice4.1 An aliquot of liquid sample or dissolved solid sample is adjusted as
10、needed to 8M nitric acid for plutonium/uranium removalusing extraction chromatography. Uranium and plutonium are retained on the resin and trace impurities are collected in the columneffluent. The impurities can be measured by a variety of techniques.1 This practice is under the jurisdiction of ASTM
11、 Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.Current edition approved July 1, 2006Jan. 1, 2013. Published August 2006January 2013. Originally approved in 2006. Last previous edition approved in 2006 as C1647 06. DOI: 10.1520/C1647-06
12、.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only t
13、o provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versiono
14、f the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Significance and Use5.1 This practice can be used to separate uranium or plutonium, or both, prior to the
15、 impurity analysis by various techniques.The removal of uranium and plutonium prior to quantification can improve the detection limits by minimizing the signalsuppression caused by uranium or plutonium when using ICP techniques. Detection limits of 110 part-per-billion (PPB) maybe obtainable by matr
16、ix removal. Also, removal of the uranium and plutonium may allow the impurities analysis to be performedon a non-glove box enclosed instrument.5.2 Other test methods exist to determine impurities in uranium or plutonium. Test Method C1517 is able to determine manyimpurities in uranium at detection l
17、evels of 110 part-per-million (ppm) by DC-Arc Spectrometry. Test Method C1287 is ableto determine impurities in uranium at detection levels of 100 ppb by ICP-MS. Test Method C1432 provides an alternativetechnique to remove plutonium by ion exchange prior to analysis of the impurities by ICP-AES.5.3
18、This practice can be used to demonstrate compliance with nuclear fuel specifications, for example, Specifications C753,C757, C776, C787, C788, and C996.6. Interferences6.1 Zirconium, hafnium, niobium, and tantalum are retained on the diamyl, amylphosphonate resin unless hydrofluoric acid isadded to
19、the nitric acid load/rinse solution. The addition of hydrofluoric acid to recover zirconium, hafnium, niobium, and tantalumreduces uranium and plutonium retention. For this reason, hydrofluoric acid levels must be minimized (typically 13 mL capacity (inner diameter = 1.5 cm has been found acceptable
20、) and reservoirs.7.2 Plastic Collection Tubes, 50 mL.7.3 Column Rack, used for gravity flow systems.7.4 Polyethylene Frits for columns, 20 m.7.5 Vacuum BoxThe use of a vacuum-assisted flow system permits the use of higher eluent flow rates. Gravity flow systemsmay be used instead.8. Reagents8.1 Puri
21、ty of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society wheresuch specifications are available.3 Other grades may be used
22、, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination. High purity acids may be used to reduce reagent blanksand to achieve lower detection limits.8.2 Purity of WaterUnless otherwise indicated, referenc
23、es to water shall be understood to mean reagent water as defined inSpecification D1193 as Type I.8.3 Hydrofluoric Acid (28 M)Concentrated hydrofluoric acid (sp gr 1.2).8.4 Nitric Acid (16 M)Concentrated HNO3 (sp gr 1.42).8.5 Nitric Acid Solution (8 M)Add 500 mL of concentrated nitric acid (sp gr 1.4
24、2) to 300 mL of water and dilute to 1 L withwater.8.6 Nitric Acid (8M)Hydrofluoric Acid (0.05M)Add 500 mLconcentrated nitric acid and 1.8 mLconcentrated hydrofluoricacid to 250 mL water and dilute to 1 liter with water.8.7 Diamyl, Amylphosphonate Resin,450100 m particle size resin for use with vacuu
25、m-assisted flow systems; 100 to 150 mor larger if using gravity flow systems.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Labor
26、atory Chemicals, BDH, Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4 The sole source of supply of only suppliers of the UTEVA resinResin known to the committee at this time is Eichrom Technologies, Inc.
27、 8205 S. Cass Ave Suite 106Darien, IL 60561. are Eichrom Technologies LLC, Lisle, IL, USA and Triskem International, Bruz, France. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receive careful consideration at a meeti
28、ng of the responsible technical committee,1 which you mayattend. This resin inis described in Horwitz, E. P., et al, “Separation and Preconcentration of Uranium fromAcidic Media by Extraction Chromatography,”Analytica ChimicaActa, 266, 1992, pp. 25-37.C1647 1328.8 Polymethacrylate Resin,5100150 m pa
29、rticle size resin.9. Hazards9.1 Refer to the laboratorys chemical hygiene plan and other applicable guidance for handling chemical and radioactivematerials and for the management of radioactive, mixed, and hazardous waste.9.2 Hydrofluoric acid is a highly corrosive acid that can severely burn skin,
30、eyes, and mucous membranes. Hydrofluoric acidis similar to other acids in that the initial extent of a burn depends on the concentration, the temperature and the duration of contactwith the acid. Hydrofluoric acid differs from other acids because the fluoride ion readily penetrates the skin causing
31、destructionof deep tissue layers. Unlike other acids that are rapidly neutralized, hydrofluoric acid reactions with tissue may continue for daysif left untreated. Due to the serious consequences of hydrofluoric acid burns, prevention of exposure or injury of personnel is theprimary goal. Utilization
32、 of appropriate laboratory controls (hoods) and wearing adequate personal protective equipment to protectfrom skin and eye contact is essential.10. Procedure10.1 Column Preparation and Conditioning:NOTE 1If prepackaged columns are available from the resin supplier, skip to 9.1.310.1.3.NOTE 2Each col
33、umn shall contain 10 mL diamyl, amylphosphonate resin. This resin amount can remove approximately 250 mg combinedplutonium/uranium to enable impurity assay by ICP-AES, ICP-MS, or AAS.10.1.1 Add approximately 3 mL of polymethacrylate resin to the bottom of a column. Rinse the column walls with water.
34、 Placea frit on top of the resin.10.1.2 Add approximately 10 mLof diamyl, amylphosphonate resin to the column. Rinse the column walls with water and placeanother frit on top of the resin.10.1.3 Place the columns on a vacuum box if using a vacuum-assisted flow system or in a column rack if using a gr
35、avity flowsystem.NOTE 3If not using a vacuum box, the larger particle size resin should be used.10.1.4 Add 10 mL 8M nitric acid to each column to condition the resin. Turn on vacuum and adjust flow rate to 24 mL/minif using a vacuum-assisted flow system. Allow each column to drain completely and tur
36、n off the vacuum if using the vacuumassisted flow system.10.1.5 Discard the eluted conditioning solutions.10.2 Column Loading and Separation:10.2.1 Procedures for dissolution of plutonium and uranium materials are found in Practices C1168 and C1347.10.2.2 Adjust the solution resulting from dissoluti
37、on so that the nitric acid concentration is 8M.10.2.3 Record the sample aliquot weight (g) or volume (mL) and sample pre-dilution factor (weight/volume or volume/volume).10.2.4 Place clean, labeled 50 mL plastic collection tubes below each column in the vacuum extraction system.10.2.5 Pipet 10 mL of
38、 sample aliquot prepared in 9.2.210.2.2 into the appropriate column. (the resin capacity is 250 mg U andPu combined. If the concentration of the sample is greater than 25 mg/mL, then less than 10 mL should be added to avoidexceeding the resin capacity).10.2.6 Turn on vacuum and adjust flow rate to 2
39、4 mL/min if using a vacuum-assisted flow system.Allow each column to draincompletely.10.2.7 Pipet 10 mL 8M nitric acid to each column and allow to drain completely.10.2.8 Repeat step 9.2.710.2.7.NOTE 4This second column elution step may be performed with hydrofluoric added (20 mL 8M HNO3 0.05M HF) t
40、o completely elute zirconium,hafnium, tantalum and niobium (see 5.16.1). This is done in a second elution rinse to minimize hydrofluoric acid in the initial column elution so thatsilicon background at the ICP-AES is minimized and silicon can be measured in the first elution. A small amount of zircon
41、ium, hafnium, tantalum andniobium may be in the first elution so results from both elutions must be added to get a final result. If silicon is not of interest, this step can be avoidedby making the 8M nitric acid load solution approximately 0.05M hydrofluoric acid.10.2.9 After columns have drained c
42、ompletely, increase the vacuum to remove residual liquid from columns, if using thevacuum-assisted flow system.10.2.10 Turn off vacuum if using the vacuum-assisted flow system and remove collection tubes from vacuum system. Adjustcollection tube volume to 30 mL with 8M nitric acid, if needed.10.2.11
43、 Submit collected fractions for analysis by the selected technique such as ICP-MS, ICP-AES, or AAS.5 The sole source of supply of the prefilteronly suppliers of the Prefilter material known to the committee at this time is Eichrom Technologies, Inc. 8205 S. Cass AveSuite 106 Darien, IL 60561. are Ei
44、chrom Technologies LLC, Lisle, IL, USAand Triskem International, Bruz, France. If you are aware of alternative suppliers, please providethis information toASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you
45、mayattend.C1647 13310.3 While not strictly within the scope of this practice, plutonium or uranium, or both, retained on the column may be elutedat this point, if desirable for the purposes of the laboratory performing this analysis. Guidance for accomplishing this may be foundin Horwitz, et al.411.
46、 Calculations11.1 Calculate the Metal Impurity, I:I 5S 2B! 3D (1)where:S = metallic impurity measured in final solution, g/mL,B = blank measurement for metallic impurity in final solution, g/mL, andD = sample dilution factor.D 5SV3PSA (2)where:SV = column removal volume, mL (typically 30 mL, step 9.
47、2.10),SA = sample aliquot used in column separation, mL (typically 10 mL, step 9.2.5), andP = pre-dilution factor (step 9.2.3).SV = column removal volume, mL (typically 30 mL, step 10.2.10),SA = sample aliquot used in column separation, mL (typically 10 mL, step 10.2.5), andP = pre-dilution factor (
48、step 10.2.3).12. Keywords12.1 AAS; extraction chromatography; ICP-AES; ICP-MS; impurities; plutonium; resin; separation; uraniumASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are
49、 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 meeting of
