1、Designation: C1517 09C1517 16Standard Test Method forDetermination of Metallic Impurities in Uranium Metal orCompounds by DC-Arc Emission Spectroscopy1This standard is issued under the fixed designation C1517; the number immediately following the designation indicates the year oforiginal adoption or
2、, 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. Scope1.1 This test method describes the steps necessary for the preparation and determin
3、ation of impurity metals in uranium metaland uranium compounds by DC arc emission spectroscopy.1.2 The method is valid for those materials that can be dissolved in acid and/oror converted to an oxide in a muffle furnacefurnace, or both (see Practice C1347).1.3 This method uses the carrier distillati
4、on technique to selectively carry the impurities into the arc, leaving the uranium oxidein the electrode. If it is necessary to determine the carrier metal(usually metal (usually a silver or strontium, or gallium compound)as an impurity, another technique must be chosen for that element.1.4 UnitsThe
5、 values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.1.5 This standard may involve hazardous materials, operations and equipment. This standard does not purport to address allof the safety concerns, if any, associated with its use. It is
6、 the responsibility of the user of this standard to establish appropriatesafety and health practices and determine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide PowderC761 Test Meth
7、ods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of UraniumHexafluorideC776 Specification for Sintered Uranium Dioxide PelletsC788 Specification for Nuclear-Grade Uranyl Nitrate Solution or CrystalsC859 Terminology Relating to Nuclear MaterialsC967 Specifica
8、tion for Uranium Ore ConcentrateC1347 Practice for Preparation and Dissolution of Uranium Materials for AnalysisE130 Practice for Designation of Shapes and Sizes of Graphite Electrodes (Withdrawn 2013)3E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials3. Termin
9、ology3.1 See definitions and terms Except as otherwise defined herein, definitions of terms are as given in Terminologies C859 andE135.4. Summary of Test Method4.1 Uranium metal, solutions and compounds are converted to uranium oxide (U3O8) in a muffle furnace. A weighed amountof the oxide is mixed
10、with an appropriate spectrographic carrier and loaded into a graphite electrode. The electrode is excited ina DC arc and the light is dispersed by a spectrograph or spectrometer. The resulting spectrum is measured electronically using a1 This test method is under the jurisdiction of ASTM Committee C
11、26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.Current edition approved June 1, 2009April 1, 2016. Published July 2009May 2016. Originally approved in 2002. Last previous edition approved in 20022009 asC1517 02.C1517 09. DOI: 10.1520/C1517-09.10.1
12、520/C1517-16.2 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.3 The last approved version of this historical s
13、tandard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to 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 r
14、ecommends that users consult prior editions as appropriate. In all cases only the current versionof 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 States1CCD, CID,
15、or CMOS camera or photographed on photographic plates or film sensitive to the proper regions. The line intensitiesare compared directly to standard plates or to calibration curves derived from the arced standards.5. Significance and Use5.1 This test method is applicable to uranium metal, uranium ox
16、ides and compounds soluble in nitric or sulfuric acid, anduranium solutions which can be converted to uranium oxide (U3O8) in a muffle furnace. It may be used to determine the impuritiesin uranium compounds as listed in Specifications C753, C776, C788, and C967.6. Apparatus6.1 Spectrograph or Spectr
17、ometerA spectrograph with sufficient resolving power and linear dispersion to separate theanalytical lines from other lines in the spectrum of the sample in the spectral region of 230.0230 to 855.0855 nm is required. Somespectrographs may be able to access wavelengths lower than 230 nm that may allo
18、w the determination of other analytes.Instruments with a reciprocal linear dispersion in the first order of 0.5 nm/mm or less are satisfactory.Adirect-reading spectrometerof comparable quality may be substituted for equipment listed, in which case the directions given by the manufacturer should besu
19、bstituted for those in this procedure.The spectrometer should include a CCD, CID, or CMOS camera for electronic measurementof the resulting spectrum.6.2 Excitation SourceUse an arc power source capable of providing a dc arc of up to 14-A dc, depending on the carrier usedand electrode design.6.3 Exci
20、tation StandConventional type with adjustable water-cooled electrode holders (may be fitted with automatic samplechangers if desired).6.4 Photographic Processing EquipmentUse developing, fixing, washing and drying equipment.6.5 Microphotometer, having a precision of at least 6 1 % for transmittances
21、.6.4 Mixer, for dry materials.6.5 Platinum Crucible.6.6 Venting Tool, (see Fig. 8, Test Methods C761). 01).6.7 Muffle Furnace, 1000C capability.7. Reagents and Materials7.1 Purity of MaterialsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreage
22、nts conform to the specifications of the Committee of Analytical Reagents of the American Chemical Society4 where suchspecifications are available. Other grades may be used provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accurac
23、y of the determination.7.2 ElectrodesThe anode and counter electrodes should be of the S-2, S 16 and C-1 types as given in Practice E130 (orequivalent).NOTE 1Exact shapes and dimensions of the electrodes are not as critical as given in Practice E130; however, dimensions of the electrodes used should
24、be consistent and it is essential that the same dimension electrodes be used for standards and samples.7.3 Photographic Processing SolutionsPrepare solutions as noted in available literature (1,2).7.4 Photographic Film/PlatesUse photo emulsion SA-1 and 1-N or equivalent.7.5 Powder Paper.7.3 Nitric A
25、cid (HNO3)concentrated (70 %), electronic grade, or equivalent.7.4 Sulfuric Acid (H2SO4)concentrated, electronic grade, or equivalent.7.5 Spectrographic CarrierThe following spectrographic carriers have been used successfully for DC Arc analysis:7.5.1 Silver Chloride-Lithium Fluoride, 11:1 w/w ratio
26、.7.5.2 Silver Chloride-Silver Fluoride, 4:1 w/w ratio.7.5.3 Gallium Oxide, 99.99 % or better.7.5.4 Silver Chloride-Strontium Fluoride, 16.4 mol % SrF2 in AgCl.7.5.5 Gallium Oxide-Lithium Fluoride, 11:1 w/w ratio.7.6 Mixing Vial, plastic, 12.7 mm (1/2 in.) by 25.4 mm (1 in.) with cap and 10 mm (3/8 i
27、n.) plastic mixing bead.4 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 Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and t
28、he United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.C1517 1627.7 Standard Uranium Oxide (U3O8) DiluentUse NBLCRM 1294 3 (or its replacement or equivalent) of known impurity levelas a diluent.8. Precautions8.1 Consult manufacturers Material S
29、afety Data Sheets (MSDS)(SDS) for chemical incompatibilities, specific hazards, or spillcleanup for any hazardous materials used in this method.8.2 All mixing and weighing operations involving uranium oxides should be carried out in properly functioning hoods orexhaust boxes.gloveboxes.9. Standardiz
30、ation and Calibration9.1 Standards:9.1.1 Standards may be synthesized by adding the impurity elements to purified U3O8 (NBL CRM 129129-A5, or equivalent)and homogenizing. Impurities in powder form, preferably as oxides, may be blended in U3O8; impurities in solution may be addedto U3O8 and the mixtu
31、re dried, blended and reignited, or the impurities and uranium may be combined in solution and reconvertedto U3O8. The individual elements should grade in such a ratio as to facilitate visual comparisons covering the desired analyticalrange for each.9.1.2 The compounds used to make U3O8 impurity sta
32、ndards should be of the highest purity available.9.1.3 Alternatively, commercially available uranium impurity standards, such as NBLCRM 1235 and 1245 series standards, maybe used. (Other standards may be available; the user should determine quality and/or applicability or applicability, or both, pri
33、orto use.) These may be supplemented by synthetic standards to extend calibration ranges, if necessary.9.1.4 For each standard used, prepare in the same ratio of uranium oxide to carrier as for samples (see Table 1 for furtherdetails).9.1.5 Charge the electrode and arc at the same conditions as dete
34、rmined to be optimum for the instrument in use.9.2 Calibration Curves:9.2.1 If a microphotometer is used, determine emulsion calibration curves and analytical curves as described in availableliterature (1,2).9.2.1 If In using a direct reading spectrometer is used, spectrometer, calibrate according t
35、o manufacturers instruction.9.2.3 For visual comparison, the darkness/width of each standard and impurity element line will establish the individual analyteconcentrations.10. Procedure10.1 Sample Preparation10.1.1 Liquid Samples:10.1.1.1 Transfer into a platinum crucible a sufficient amount of liqui
36、d to yield not more than 2 g uranium oxide.10.1.1.2 Place the crucible on a hot plate and evaporate to dryness. Do not allow to boil.NOTE 2The addition of H2SO4 may be necessary for solutions of uranyl chloride to effect complete conversion to oxide.10.1.1.3 Continue the preparation at 10.1.2.2.10.1
37、.2 Miscellaneous Uranium Oxides, Solids or Compounds:10.1.2.1 Transfer not more than 2 g of the uranium compound to a platinum crucible.10.1.2.2 Place in a cool muffle and set the muffle to 900 6 50C.5 Available from the US Department of Energy, New Brunswick Laboratory, D350, Building 350, 9800 Sou
38、th CassAvenue,Argonne, IL60439,ATTN: Reference MaterialSales. http:/www.nbl.doe.gov/http:/science.energy.gov/nbl/.TABLE 1 CarrierSample CombinationsCarrierMaterialCarrier Wt,(mg)Oxide Wt,(mg)ElectrodeCharge, (mg)Mixing Time,(s)AgCl/AgF(4:1)50 250 50 180AgCl/LiF(11:1)30 270 100 60AgCl/SrF2(6:1)50 450
39、 100 30Ga2O3/LiF(11:1)20 380 100 25Ga2O3A 7 343 100 60A For the determination of Ag and Li only.C1517 163NOTE 3Some impurities (for example, Mo, W, Cr) may be lost at high temperatures. Do NOT place samples directly in hot muffle. Lowertemperatures may be used if it is determined that complete oxide
40、 conversion is achieved.10.1.2.3 Leave the crucibles and samples in the muffle until conversion to U3O8 is complete.NOTE 4Times will vary depending on amount and type of sample; the user must determine optimum time experimentally for histheir sample types.NOTE 1The above listed combinations of carri
41、er, uranium oxide andelectrode charge have been successfully used for the determination ofimpurities in uranium oxide. Other combinations may be available orsuitable. However, the user must demonstrate comparable precision andbias.TABLE 2 Typical Wavelengths and Limits of DetectionElement Wavelength
42、(nm)LOD usingAgCl/AgF(ppm)LOD usingAgCl/LiF(ppm)LOD usingGa2O3/LiF(ppm)Al 308.21236.701 5 1As 234.98 10 . . .Au 267.59 1 . . .B 249.77 0.1 0.4 0.5Ba 455.40493.412 1Be 234.86249.450.1 1 1Bi 306.77 1 . . .Ca 396.84422.6410 25Cd 228.80 0.1 0.3 0.5Co 240.72340.511 5Cr 284.33425.44427.482 10 3Cs 852.11 1
43、0 . . .Cu 324.75327.401 2 1Fe 248.33252.28302.0610 20 2Ga 294.36 1 . . .Ge 265.12 1 . . .K 769.89 10 . . .Li 670.78 0.2Mg 279.55280.272 10 1Mn 279.48279.831 10 1Mo 313.21 10Na 588.99589.591 10Nb 316.34 10 . . .Ni 300.25341.481 5 2P 255.33213.62100 25Pb 283.31 4 3 1Pd 340.46 1 . . .Rb 780.02 20 . . .
44、Sb 259.81 2 10Si 250.69251.61288.1610 10 1Sn 283.99317.5010 2 1Sr 407.77 20 . . .Ta 265.33 35Ti 334.90337.284 5V 292.40318.341 5W 294.70 100 . . .Zn 330.25213.8610 10 30C1517 16410.2 Addition of Carrier:10.2.1 Weigh an appropriate amount of uranium oxide into a mixing vial and add the amount of carr
45、ier chosen (see Table 1).10.2.2 Mix on a mixer for at least 1 min.NOTE 5Exact time will depend on efficiency of mixing action of the mixer chosen, the amount of sample and carrier used. The user must determinethis experimentally for histheir sample type (see Table 1).10.3 Charge each electrode with
46、the amount of uranium oxide and carrier determined to be optimum. For each sample chargeduplicate electrodes.10.4 Grip each electrode with forceps and pack the charge by tapping on a solid surface.10.5 Further compress and vent the charge with the venting tool shortly before arcing the samples. Wipe
47、 the venting tool withtissue between different samples.NOTE 6Venting is dependent on the carrier used and may not be required. A combination tamping/venting tool is permissible.10.6 Arc the electrodes at the conditions determined optimum for the instrument in use.10.7 If photographic film or plates
48、are used, process as directed in available literature (In using 1,2). If a direct readingspectrograph is used, the impurity values will be reportedspectrograph, the sample emission spectra will be acquired as eachelectrode is arced.10.8 Determine each impurity by comparing the lines for each element
49、 using the calibration curves established in 9.2.11. Precision and Bias11.1 Within the different stages of the nuclear fuel cycle many challenges lead to the inability to perform interlaboratory studiesfor precision and bias. These challenges may include variability of matrices of material tested, lack of suitable reference orcalibration materials, limited laboratories performing testing, shipment of materials to be tested, and regulatory constraints.Because of these challenges each laboratory utilizing these test methods should develop their ow
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