ASTM C1432-2003(2008) Standard Test Method for Determination of Impurities in Plutonium Acid Dissolution Ion Exchange Matrix Separation and Inductively Coupled Plasma-Atomic Emissi.pdf

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1、Designation: C 1432 03 (Reapproved 2008)Standard Test Method forDetermination of Impurities in Plutonium: Acid Dissolution,Ion Exchange Matrix Separation, and Inductively CoupledPlasma-Atomic Emission Spectroscopic (ICP/AES) Analysis1This standard is issued under the fixed designation C 1432; the nu

2、mber immediately following the designation indicates the year oforiginal adoption or, in the 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. Scop

3、e1.1 This test method covers the determination of 25 ele-ments in plutonium (Pu) materials. The Pu is dissolved in acid,the Pu matrix is separated from the target impurities by an ionexchange separation, and the concentrations of the impuritiesare determined by inductively coupled plasma-atomic emis

4、sionspectroscopy (ICP-AES).1.2 This test method is specific for the determination ofimpurities in8MHNO3solutions. Impurities in other pluto-nium materials, including plutonium oxide samples, may bedetermined if they are appropriately dissolved (see PracticeC 1168) and converted to8MHNO3solutions.1.3

5、 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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-p

6、riate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C 757 Specification for Nuclear-Grade Plutonium DioxidePowder, SinterableC 758 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear,

7、and Radiochemical Analysis ofNuclear-Grade Plutonium MetalC 759 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC 1168 Practice for Preparation and Dissolution of Pluto-nium Materials for AnalysisD 1193 Spe

8、cification for Reagent Water3. Summary of Test Method3.1 A sample of plutonium metal is dissolved in a smallvolume of 6 M hydrochloric acid (HCl). Then, 10 M (HNO3)/0.03 M hydrofluoric acid (HF) is added to the dissolvedplutonium to oxidize the plutonium to the Pu (IV) state. Thesample solution is l

9、oaded onto a nitrate anion exchange resinand eluted with8MHNO3/0.006 M HF. The rinses contain thetarget metallic impurities and less than 15 g/mL Pu. Theplutonium is stripped from the anion exchange resin with 0.1M HCl. The rinses containing the metallic impurities areanalyzed by ICP-AES.4. Signific

10、ance and Use4.1 This test method can be used on plutonium matrices innitrate solutions.4.2 This test method has been validated for all elementslisted in Test Methods C 757 except sulfur (S) and tantalum(Ta).4.3 This test method has been validated for all of the cationelements measured in Table 1. Ph

11、osphorus (P) requires avacuum or an inert gas purged optical path instrument.5. Interferences5.1 Plutonium concentrations of less than 50 g/mL in thefinal aqueous phase do not significantly affect the analyticalresults for most elements. Interference studies should be madeto determine the degree of

12、Pu and other elemental interferenceson the target analytes; background and interelement correctionsmay be required.1This test method is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved

13、 Dec. 1, 2008. Published January 2009. Originallyapproved in 1999. Last previous edition approved in 2003 as C 1432 03.2For 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

14、to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 An ICP-AES equipped with a Charge Injection Device(CID) detector or an ICP-AES with a spectral bandpass of 0.05

15、nm or less is required to provide the necessary spectralresolution.3The spectrometer may be either a simultaneousmultielement or a sequential spectrometer. The spectrometermay be either an inert gas-path or vacuum instrument; theappropriate spectral lines should be selected for each specificinstrume

16、nt. Either an analog or digital readout system may beused.6.2 The ICP-AES is interfaced to a glovebox. The torch boxis glovebox enclosed, since plutonium containing materialscome in direct contact with the torch. This setup is described inASTM STP 951.46.3 Vacuum manifold set at approximately 23 cm

17、Hg (9 in.Hg) is optional.5A gravity system is also acceptable.6.4 15 mL plastic disposable ion exchange columns.66.5 50 mL plastic vials.6.6 Plastic micro and macro pipettes.6.7 1000 mL plastic volumetric flasks.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in a

18、ll tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society(ACS), where such specifications are available.7Other gradescould be used, provided it is first ascertained that the reag

19、ent isof sufficiently high purity to permit its use without lesseningthe accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean laboratory accepteddemineralized or deionized water as described by Type 1 ofSpecification D 1193.7.3 U

20、ltra high purity acids shall be used for sample disso-lution and calibration standards preparation unless otherwisenoted.3The sole source of supply of the apparatus known to the committee at this timeis Thermo Jarrell Ash PolyScan Iris spectrometer (Thermo Electron Spectroscopy,Franklin, MA), or an

21、Applied Research Laboratories 3580 ICP-AES instrument(Dearborn, MI). If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.

22、4Edellson, M. C., and Daniel, J. Leland, “Plasma Spectroscopy of the Analysisof Hazardous Materials: Design and Application of Enclosed Plasma Sources,”Conference Proceedings, ASTM STP 951, ASTM, 1986.5The sole source of supply of the apparatus known to the committee at this timeis Eichrom Technolog

23、ies Vacuum Box System (Part # AC-24-BOX), EichromTechnologies Inc., Darien. IL. If you are aware of alternative suppliers, pleaseprovide this information to ASTM International Headquarters. Your comments willreceive careful consideration at a meeting of the responsible technical committee,1which you

24、 may attend.6The sole source of supply of the apparatus known to the committee at this timeis Ion exchange columns from either Applied Separation or Bio-Rad Inc. If you areaware of alternative suppliers, please provide this information to ASTM Interna-tional Headquarters. Your comments will receive

25、careful consideration at a meetingof the responsible technical committee,1which you may attend.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Sta

26、ndards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Percent Recovery and Repeatability Standard Deviation for Sixteen Spiked SamplesElementWavelength/Order(nm)Actual

27、Conc(g/mL)Mean Conc(g/mL)Average(%R)R.S.D.(%)Aluminum Al 396.152 67 2.5 2.4 95 6Barium Ba 455.403 58 2.5 2.4 95 5Beryllium Be 313.042 84 2.5 2.3 94 6Boron B 249.773 106 2.5 2.5 100 7Cadmium Cd 226.502 116 2.5 2.5 101 12Calcium Ca 396.847 66 2.5 2.6 104 20Chromium Cr 283.563 93 2.5 2.3 92 8Cobalt Co

28、228.616 115 2.5 2.5 101 6Copper Cu 324.754 81 2.5 2.4 97 6Iron Fe 259.940 101 2.5 2.5 101 12Lead Pb 220.353 120 2.5 3.1 122 12Lithium Li 670.784 39 2.5 2.2 87 6Magnesium Mg 280.270 94 2.5 2.4 95 6Manganese Mn 257.610 102 2.5 2.5 98 5Molybdenum Mo 202.030 130 2.5 2.6 103 10Nickel Ni 231.604 114 2.5 2

29、.5 100 11Silicon Si 251.612 104 2.5 2.3 92 16Sodium Na 588.995 45 25.0 24.7 97 16Strontium Sr 421.552 62 2.5 2.4 95 5Tin Sn 189.989 139 2.5 2.7 109 19Titanium Ti 334.941 79 2.5 2.5 102 8Tungsten W 207.911 127 2.5 2.5 99 11Vanadium V 292.402 90 2.5 2.0 82 7Zinc Zn 213.856 123 2.5 2.5 100 8Zirconium Z

30、r 339.198 78 2.5 2.5 101 10C 1432 03 (2008)2NOTE 1The molarity of ultra high purity acids may vary fromstandard ACS specifications for concentrated acids.NOTE 2All reagents are prepared and stored in polytetrafluoroethyl-ene (PTFE) containers.7.4 Hydrochloric Acid (HCl, 11.3 M), concentrated ultrahi

31、gh purity8HCl.7.5 Hydrochloric Acid (HCl, 6 M)Add 531 mL of con-centrated ultra high purity HCl (11.3 M) to less than 450 mL ofwater and dilute to 1 L with water.7.6 Hydrochloric Acid (HCl, 0.1 M)Add 8.8 mL ofconcentrated ultra high purity HCl (11.3 M) to water, whilestirring, and dilute to 1 L with

32、 water. (Reagent grade HCl canbe used in preparing this reagent.)7.7 Hydrofluoric Acid (HF, 28.3 M), concentrated ultra highpurity8HF.7.8 Nitric Acid (HNO3, 15.8 M), concentrated ultra highpurity8nitric acid.7.9 Nitric Acid-Hydrofluoric Acid Mixture,10MHNO3/0.03 M HFAdd 1 mL of concentrated ultra hi

33、gh purity HF(28.3 M) to water; using a plastic pipette, while stirring, add633 mL concentrated ultra high purity HNO3(15.8 M) anddilute to 1 L with water.7.10 Nitric Acid-Hydrofluoric Acid Mixture,8MHNO3/0.006 M HFAdd 0.21 mL of concentrated ultra high purityHF (28.3 M) to water; using a plastic pip

34、ette, while stirring,add 506 mL of concentrated ultra high purity HNO3(15.8 M)and dilute to 1 L with water.7.11 Nitric Acid (HNO3,4M)Add 253 mL of concen-trated ultra high purity nitric acid (15.8 M) to water, whilestirring, and dilute to 1 L with water.7.12 Anion Exchange Resin, macroporous-1 (MP-1

35、), 200-400 mesh, either nitrate form or chloride form, high purity.97.13 Stock Solutions, traceable to a national standard, ofmultielement spike solutions are available from a commercialvendor. The stock solutions of multielement spike solutionscan also be prepared in-house.7.13.1 Spike Solution 1 (

36、SS-1), contains 500 g/mL of Al,Ba, Be, Ca, Li, Mg, Sr, and Na in 0.8 M HNO3.107.13.2 Spike Solution 2 (SS-2), contains 500 g/mL of B,Mo, Si, Sn, Ti, W, and Zr in 0.8 M HNO3.107.13.3 Spike Solution 3 (SS-3), contains 500 g/mL of Cd,Cr, Co, Cu, Fe, Pb, Mn, Ni, V, and Zn in 0.8 M HNO3.107.14 Stock Solu

37、tions, traceable to a national standard, ofmultielement impurity standards are available from a commer-cial vendor. The stock solutions of multielement standards canalso be prepared in-house.7.14.1 Calibration Stock Solution-2 (CSS-2), contains 5000g/mL of Na in 0.8 M HNO3.117.14.2 Calibration Stock

38、 Solution-3 (CSS-3), contains 500g/mLof Mo, Si, Sn, Ti, W, and Zr in 0.3 M HNO3/0.1 M HF.117.14.3 Calibration Stock Solution-5 (CSS-5), contains 500g/mL of Al, Ba, and Sr in 0.8 M HNO3.117.14.4 Calibration Stock Solution-6 (CSS-6), contains 500g/mL of Be, B, Cd, Ca, Cr, Co, Cu, Fe, Li, Mg, Mn, Ni, P

39、b,V, and Zn in 0.8 M HNO3.117.15 Prepare the multielement impurity standards andblanks as described in 7.15.1-7.15.5. All calibration standardsolutions are stored in PTFE containers.7.15.1 Calibration Standard One High (CAL 1 HI)Pipette20 mL each, of stock solutions CSS-3, and CSS-5 into a 1 Lvolume

40、tric flask. Dilute to 1 L with8MHNO3/0.006 M HF.This standard solution contains the target analytes at a concen-tration of 10 g/mL.7.15.2 Calibration Standard One Low (CAL 1 LO)Pipette10 mL each, of stock solutions CSS-3, and CSS-5 into a 1 Lvolumetric flask. Dilute to 1 L with8MHNO3/0.006 M HF.This

41、 standard solution contains the target analytes at a concen-tration of 5 g/mL.7.15.3 Calibration Standard Two High (CAL 2 HI)Pipette20 mL each, of stock solutions CCS-2, and CSS-6 intoa1Lvolumetric flask. Dilute to 1 L with8MHNO3/0.006 M HF.This standard solution contains the target analytes at a co

42、ncen-tration of 10 g/mL, except Na. Na is 100 g/mL.7.15.4 Calibration Standard Two Low (CAL 2 LO)Pipette10 mL each, of stock solutions CCS-2, and CCS-6 intoa1Lvolumetric flask. Dilute to 1 L with8MHNO3/0.006 M HF.This standard solution contains the target analytes at a concen-tration of 5 g/mL, exce

43、pt Na. Na is 50 g/mL.7.15.5 Calibration Standard Blank (CAL BL)This blankis an 8 M HNO3/0.006 M HF solution.8. Hazards8.1 Plutonium bearing materials are radioactive and toxic.Adequate laboratory facilities, gloveboxes and fume hoodsalong with safe techniques, must be used in handling samplescontain

44、ing these materials. A detailed discussion of all theprecautions necessary is beyond the scope of this test method;however, personnel who handle these materials should befamiliar with such safe handling practices.9. Procedure9.1 Preparation of Anion Exchange Resin Slurry:9.1.1 If the anion exchange

45、resin was purchased in thenitrate form, prepare a 1:1 (volume:volume) slurry of the resinin 4 M HNO3and proceed to 9.2.9.1.2 If the anion resin was purchased in the chloride form,convert it to the nitrate form.8The sole source of supply of the apparatus known to the committee at this timeis Ultrex (

46、J. T. Baker, Inc.) and Seastar brands of ultra high purity acids. If you areaware of alternative suppliers, please provide this information to ASTM Interna-tional Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.9

47、The sole source of supply of the apparatus known to the committee at this timeis AG MP-1 anion exchange resin, Bio-Rad, Richmond, CA. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a mee

48、ting of theresponsible technical committee,1which you may attend.10The sole source of supply of the apparatus known to the committee at this timeis Multielement spike solutions, Inorganic Ventures, NJ. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHea

49、dquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.11The sole source of supply of the apparatus known to the committee at this timeis Multielement impurity standards, High Purity, SC. 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.C 1432 03